# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-Co
_database_code_depnum_ccdc_archive 'CCDC 2265688'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2023-05-26 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C82 H114 Ca2 Co2 N4 O4, 2(C6 H14)'
_chemical_formula_sum            'C94 H142 Ca2 Co2 N4 O4'
_chemical_formula_weight         1590.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.6568(4)
_cell_length_b                   13.2884(3)
_cell_length_c                   19.2033(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.9516(19)
_cell_angle_gamma                90
_cell_volume                     4505.07(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6460
_cell_measurement_theta_min      4.0190
_cell_measurement_theta_max      72.6720

_exptl_crystal_description       blocks
_exptl_crystal_colour            'Light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_F_000             1720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.085
_exptl_absorpt_coefficient_mu    4.255
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            26645
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.373
_diffrn_reflns_theta_max         73.863
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8902
_reflns_number_gt                6565
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0820P)²+0.4814P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8902
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1477
_refine_ls_wR_factor_gt          0.1333
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.48907(3) 0.44585(4) 0.40977(2) 0.04506(13) Uani 1 1 d . . . . .
Co1 Co 0.64581(3) 0.74204(3) 0.46575(2) 0.05389(14) Uani 1 1 d . . . . .
N1 N 0.43134(12) 0.54556(15) 0.32395(11) 0.0476(5) Uani 1 1 d . . . . .
C1 C 0.46400(16) 0.58350(19) 0.26789(13) 0.0511(6) Uani 1 1 d . . . . .
C2 C 0.53393(16) 0.5522(2) 0.24208(14) 0.0541(6) Uani 1 1 d . . . . .
H2 H 0.553389 0.593932 0.206402 0.065 Uiso 1 1 calc R U . . .
C3 C 0.58034(15) 0.46974(19) 0.25984(13) 0.0507(6) Uani 1 1 d . . . . .
N3 N 0.57155(12) 0.41235(15) 0.31563(11) 0.0475(5) Uani 1 1 d . . . . .
C4 C 0.42452(19) 0.6663(2) 0.22620(16) 0.0665(8) Uani 1 1 d . . . . .
H4A H 0.370420 0.650766 0.221506 0.100 Uiso 1 1 calc R U . . .
H4B H 0.446747 0.670654 0.179875 0.100 Uiso 1 1 calc R U . . .
H4C H 0.430996 0.730725 0.250396 0.100 Uiso 1 1 calc R U . . .
C5 C 0.64358(18) 0.4499(2) 0.20894(15) 0.0629(7) Uani 1 1 d . . . . .
H5A H 0.686957 0.493154 0.220437 0.094 Uiso 1 1 calc R U . . .
H5B H 0.625565 0.464531 0.161473 0.094 Uiso 1 1 calc R U . . .
H5C H 0.659000 0.379167 0.212091 0.094 Uiso 1 1 calc R U . . .
C6 C 0.35455(15) 0.5744(2) 0.33852(13) 0.0512(6) Uani 1 1 d . . . . .
C7 C 0.29580(17) 0.5094(2) 0.31641(15) 0.0607(7) Uani 1 1 d . . . . .
C8 C 0.22147(18) 0.5353(3) 0.33232(19) 0.0744(9) Uani 1 1 d . . . . .
H8 H 0.181152 0.492977 0.316948 0.089 Uiso 1 1 calc R U . . .
C9 C 0.20531(18) 0.6205(3) 0.36971(19) 0.0762(9) Uani 1 1 d . . . . .
H9 H 0.154278 0.636911 0.379751 0.091 Uiso 1 1 calc R U . . .
C10 C 0.26313(17) 0.6820(3) 0.39253(17) 0.0674(8) Uani 1 1 d . . . . .
H10 H 0.251504 0.740276 0.418922 0.081 Uiso 1 1 calc R U . . .
C11 C 0.33905(16) 0.6605(2) 0.37769(14) 0.0548(6) Uani 1 1 d . . . . .
C12 C 0.3122(2) 0.4146(3) 0.27416(18) 0.0722(8) Uani 1 1 d . . . . .
H12 H 0.364852 0.392730 0.286591 0.087 Uiso 1 1 calc R U . . .
C13 C 0.2595(2) 0.3273(3) 0.2911(2) 0.0967(12) Uani 1 1 d . . . . .
H13A H 0.259619 0.316210 0.341586 0.145 Uiso 1 1 calc R U . . .
H13B H 0.277003 0.266207 0.267742 0.145 Uiso 1 1 calc R U . . .
H13C H 0.207925 0.343268 0.274950 0.145 Uiso 1 1 calc R U . . .
C14 C 0.3103(3) 0.4371(4) 0.1964(2) 0.1039(14) Uani 1 1 d . . . . .
H14A H 0.260523 0.464211 0.183086 0.156 Uiso 1 1 calc R U . . .
H14B H 0.319584 0.374977 0.170428 0.156 Uiso 1 1 calc R U . . .
H14C H 0.349583 0.486575 0.185746 0.156 Uiso 1 1 calc R U . . .
C15 C 0.40040(17) 0.7298(2) 0.40529(15) 0.0581(7) Uani 1 1 d . . . . .
H15 H 0.449255 0.709302 0.383813 0.070 Uiso 1 1 calc R U . . .
C16 C 0.3851(2) 0.8396(2) 0.3857(2) 0.0783(9) Uani 1 1 d . . . . .
H16A H 0.380322 0.845542 0.334928 0.117 Uiso 1 1 calc R U . . .
H16B H 0.427095 0.881702 0.402499 0.117 Uiso 1 1 calc R U . . .
H16C H 0.337914 0.861893 0.407061 0.117 Uiso 1 1 calc R U . . .
C17 C 0.40989(19) 0.7212(3) 0.48427(16) 0.0691(8) Uani 1 1 d . . . . .
H17A H 0.415690 0.650301 0.497260 0.104 Uiso 1 1 calc R U . . .
H17B H 0.365095 0.749120 0.506750 0.104 Uiso 1 1 calc R U . . .
H17C H 0.454958 0.758819 0.499485 0.104 Uiso 1 1 calc R U . . .
C18 C 0.61755(15) 0.32421(19) 0.32560(13) 0.0512(6) Uani 1 1 d . . . . .
C19 C 0.69117(16) 0.3313(2) 0.35501(15) 0.0579(7) Uani 1 1 d . . . . .
C20 C 0.7299(2) 0.2420(2) 0.37035(18) 0.0694(8) Uani 1 1 d . . . . .
H20 H 0.779009 0.245608 0.391138 0.083 Uiso 1 1 calc R U . . .
C21 C 0.6991(2) 0.1497(3) 0.35629(18) 0.0739(9) Uani 1 1 d . . . . .
H21 H 0.726559 0.090153 0.367198 0.089 Uiso 1 1 calc R U . . .
C22 C 0.6281(2) 0.1437(2) 0.32627(18) 0.0727(9) Uani 1 1 d . . . . .
H22 H 0.607100 0.079345 0.316168 0.087 Uiso 1 1 calc R U . . .
C23 C 0.58597(18) 0.2297(2) 0.31026(16) 0.0612(7) Uani 1 1 d . . . . .
C24 C 0.73035(17) 0.4315(2) 0.36963(17) 0.0655(7) Uani 1 1 d . . . . .
H24 H 0.695828 0.486442 0.352971 0.079 Uiso 1 1 calc R U . . .
C25 C 0.8045(2) 0.4398(3) 0.3293(2) 0.0862(11) Uani 1 1 d . . . . .
H25A H 0.826819 0.506491 0.337007 0.129 Uiso 1 1 calc R U . . .
H25B H 0.793952 0.430268 0.279497 0.129 Uiso 1 1 calc R U . . .
H25C H 0.839985 0.387980 0.345757 0.129 Uiso 1 1 calc R U . . .
C26 C 0.7458(2) 0.4479(3) 0.44740(19) 0.0778(9) Uani 1 1 d . . . . .
H26A H 0.698316 0.441836 0.472759 0.117 Uiso 1 1 calc R U . . .
H26B H 0.767164 0.515195 0.454790 0.117 Uiso 1 1 calc R U . . .
H26C H 0.781846 0.397144 0.464478 0.117 Uiso 1 1 calc R U . . .
C27 C 0.5085(2) 0.2216(2) 0.27485(19) 0.0729(9) Uani 1 1 d . . . . .
H27 H 0.478750 0.282282 0.288678 0.087 Uiso 1 1 calc R U . . .
C28 C 0.4630(3) 0.1280(3) 0.2975(3) 0.1044(14) Uani 1 1 d . . . . .
H28A H 0.487355 0.067097 0.279688 0.157 Uiso 1 1 calc R U . . .
H28B H 0.411191 0.132402 0.278601 0.157 Uiso 1 1 calc R U . . .
H28C H 0.461644 0.125047 0.348420 0.157 Uiso 1 1 calc R U . . .
C29 C 0.5158(3) 0.2246(4) 0.1953(2) 0.1051(14) Uani 1 1 d . . . . .
H29A H 0.544926 0.284141 0.182019 0.158 Uiso 1 1 calc R U . . .
H29B H 0.465194 0.227792 0.173629 0.158 Uiso 1 1 calc R U . . .
H29C H 0.541824 0.163830 0.179580 0.158 Uiso 1 1 calc R U . . .
C31 C 0.70740(18) 0.7729(2) 0.37498(16) 0.0605(7) Uani 1 1 d . . . . .
C32 C 0.75300(18) 0.7952(3) 0.43506(18) 0.0698(8) Uani 1 1 d . . . . .
C33 C 0.7148(2) 0.8704(2) 0.47384(18) 0.0705(9) Uani 1 1 d . . . . .
C34 C 0.6461(2) 0.8960(2) 0.43799(17) 0.0677(8) Uani 1 1 d . . . . .
C35 C 0.64116(19) 0.8362(2) 0.37702(16) 0.0619(7) Uani 1 1 d . . . . .
C36 C 0.7246(2) 0.7036(2) 0.31716(17) 0.0725(9) Uani 1 1 d . . . . .
H36A H 0.761468 0.653143 0.333240 0.109 Uiso 1 1 calc R U . . .
H36B H 0.745868 0.741773 0.278433 0.109 Uiso 1 1 calc R U . . .
H36C H 0.678046 0.669847 0.301479 0.109 Uiso 1 1 calc R U . . .
C37 C 0.8284(2) 0.7500(3) 0.4523(2) 0.0914(12) Uani 1 1 d . . . . .
H37A H 0.833573 0.741635 0.502868 0.137 Uiso 1 1 calc R U . . .
H37B H 0.868576 0.794396 0.435753 0.137 Uiso 1 1 calc R U . . .
H37C H 0.832551 0.684179 0.429617 0.137 Uiso 1 1 calc R U . . .
C38 C 0.7433(3) 0.9161(3) 0.5405(2) 0.1031(14) Uani 1 1 d . . . . .
H38A H 0.700342 0.931375 0.570394 0.155 Uiso 1 1 calc R U . . .
H38B H 0.770876 0.978212 0.530366 0.155 Uiso 1 1 calc R U . . .
H38C H 0.777276 0.868538 0.564384 0.155 Uiso 1 1 calc R U . . .
C39 C 0.5901(3) 0.9718(3) 0.4625(2) 0.0910(12) Uani 1 1 d . . . . .
H39A H 0.542755 0.964709 0.435591 0.136 Uiso 1 1 calc R U . . .
H39B H 0.610544 1.039621 0.455960 0.136 Uiso 1 1 calc R U . . .
H39C H 0.580286 0.960707 0.511971 0.136 Uiso 1 1 calc R U . . .
C40 C 0.5805(2) 0.8393(3) 0.32176(17) 0.0725(9) Uani 1 1 d . . . . .
H40A H 0.569419 0.770799 0.305710 0.109 Uiso 1 1 calc R U . . .
H40B H 0.597698 0.880001 0.282502 0.109 Uiso 1 1 calc R U . . .
H40C H 0.534543 0.869279 0.340857 0.109 Uiso 1 1 calc R U . . .
C41 C 0.59548(15) 0.63036(19) 0.43899(14) 0.0503(6) Uani 1 1 d . . . . .
H41 H 0.597672 0.617365 0.390419 0.060 Uiso 1 1 calc R U . . .
O41 O 0.55671(10) 0.56397(12) 0.47314(9) 0.0466(4) Uani 1 1 d . . . . .
C42 C 0.6181(2) 0.7180(3) 0.54705(16) 0.0695(8) Uani 1 1 d . . . . .
O42 O 0.59118(18) 0.6975(2) 0.59870(13) 0.0994(9) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O41 2.3070(17) . ?
Ca1 N1 2.336(2) . ?
Ca1 O42 2.378(2) 3_666 ?
Ca1 N3 2.382(2) . ?
Ca1 O41 2.4054(17) 3_666 ?
Co1 C42 1.675(3) . ?
Co1 C41 1.800(3) . ?
Co1 C33 2.100(3) . ?
Co1 C31 2.110(3) . ?
Co1 C32 2.113(3) . ?
Co1 C34 2.114(3) . ?
Co1 C35 2.114(3) . ?
N1 C1 1.329(3) . ?
N1 C6 1.441(3) . ?
C1 C2 1.401(4) . ?
C1 C4 1.523(4) . ?
C2 C3 1.407(4) . ?
C3 N3 1.326(3) . ?
C3 C5 1.519(4) . ?
N3 C18 1.436(3) . ?
C6 C11 1.399(4) . ?
C6 C7 1.410(4) . ?
C7 C8 1.396(5) . ?
C7 C12 1.528(5) . ?
C8 C9 1.374(5) . ?
C9 C10 1.374(5) . ?
C10 C11 1.404(4) . ?
C11 C15 1.511(4) . ?
C12 C14 1.522(5) . ?
C12 C13 1.526(5) . ?
C15 C17 1.527(4) . ?
C15 C16 1.530(4) . ?
C18 C23 1.403(4) . ?
C18 C19 1.412(4) . ?
C19 C20 1.398(4) . ?
C19 C24 1.525(4) . ?
C20 C21 1.367(5) . ?
C21 C22 1.373(5) . ?
C22 C23 1.396(4) . ?
C23 C27 1.521(5) . ?
C24 C26 1.529(5) . ?
C24 C25 1.536(4) . ?
C27 C29 1.535(6) . ?
C27 C28 1.548(5) . ?
C31 C32 1.427(5) . ?
C31 C35 1.441(5) . ?
C31 C36 1.478(4) . ?
C32 C33 1.423(5) . ?
C32 C37 1.493(5) . ?
C33 C34 1.426(5) . ?
C33 C38 1.496(5) . ?
C34 C35 1.417(4) . ?
C34 C39 1.493(5) . ?
C35 C40 1.496(5) . ?
C41 O41 1.301(3) . ?
C42 O42 1.140(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O41 Ca1 N1 101.67(7) . . ?
O41 Ca1 O42 152.09(8) . 3_666 ?
N1 Ca1 O42 98.83(9) . 3_666 ?
O41 Ca1 N3 102.11(7) . . ?
N1 Ca1 N3 80.54(7) . . ?
O42 Ca1 N3 99.76(9) 3_666 . ?
O41 Ca1 O41 73.91(6) . 3_666 ?
N1 Ca1 O41 122.74(7) . 3_666 ?
O42 Ca1 O41 79.13(8) 3_666 3_666 ?
N3 Ca1 O41 156.69(7) . 3_666 ?
C42 Co1 C41 87.60(13) . . ?
C42 Co1 C33 105.32(14) . . ?
C41 Co1 C33 166.79(12) . . ?
C42 Co1 C31 165.90(15) . . ?
C41 Co1 C31 100.55(11) . . ?
C33 Co1 C31 66.23(12) . . ?
C42 Co1 C32 126.93(15) . . ?
C41 Co1 C32 129.49(13) . . ?
C33 Co1 C32 39.47(13) . . ?
C31 Co1 C32 39.50(13) . . ?
C42 Co1 C34 114.94(15) . . ?
C41 Co1 C34 136.81(13) . . ?
C33 Co1 C34 39.56(14) . . ?
C31 Co1 C34 66.43(12) . . ?
C32 Co1 C34 66.45(14) . . ?
C42 Co1 C35 148.89(16) . . ?
C41 Co1 C35 104.20(12) . . ?
C33 Co1 C35 66.05(13) . . ?
C31 Co1 C35 39.91(12) . . ?
C32 Co1 C35 66.46(13) . . ?
C34 Co1 C35 39.15(12) . . ?
C1 N1 C6 118.6(2) . . ?
C1 N1 Ca1 126.63(17) . . ?
C6 N1 Ca1 114.51(15) . . ?
N1 C1 C2 124.8(2) . . ?
N1 C1 C4 119.9(2) . . ?
C2 C1 C4 115.3(2) . . ?
C1 C2 C3 131.2(2) . . ?
N3 C3 C2 124.6(2) . . ?
N3 C3 C5 121.1(2) . . ?
C2 C3 C5 114.2(2) . . ?
C3 N3 C18 120.2(2) . . ?
C3 N3 Ca1 125.93(17) . . ?
C18 N3 Ca1 113.74(15) . . ?
C11 C6 C7 120.9(3) . . ?
C11 C6 N1 121.0(2) . . ?
C7 C6 N1 117.9(2) . . ?
C11 C6 Ca1 110.85(16) . . ?
C7 C6 Ca1 109.72(18) . . ?
N1 C6 Ca1 41.41(11) . . ?
C8 C7 C6 118.2(3) . . ?
C8 C7 C12 120.4(3) . . ?
C6 C7 C12 121.4(3) . . ?
C9 C8 C7 121.5(3) . . ?
C10 C9 C8 119.8(3) . . ?
C9 C10 C11 121.4(3) . . ?
C6 C11 C10 118.1(3) . . ?
C6 C11 C15 122.8(2) . . ?
C10 C11 C15 119.1(3) . . ?
C14 C12 C13 110.8(3) . . ?
C14 C12 C7 111.0(3) . . ?
C13 C12 C7 113.1(3) . . ?
C11 C15 C17 111.7(3) . . ?
C11 C15 C16 111.8(2) . . ?
C17 C15 C16 109.3(3) . . ?
C23 C18 C19 120.2(3) . . ?
C23 C18 N3 118.7(3) . . ?
C19 C18 N3 120.9(2) . . ?
C23 C18 Ca1 105.79(18) . . ?
C19 C18 Ca1 114.53(17) . . ?
N3 C18 Ca1 42.31(11) . . ?
C20 C19 C18 118.2(3) . . ?
C20 C19 C24 118.9(3) . . ?
C18 C19 C24 122.9(2) . . ?
C21 C20 C19 121.9(3) . . ?
C20 C21 C22 119.5(3) . . ?
C21 C22 C23 121.6(3) . . ?
C22 C23 C18 118.6(3) . . ?
C22 C23 C27 120.8(3) . . ?
C18 C23 C27 120.6(3) . . ?
C19 C24 C26 112.2(3) . . ?
C19 C24 C25 111.0(3) . . ?
C26 C24 C25 110.0(3) . . ?
C23 C27 C29 110.7(3) . . ?
C23 C27 C28 113.5(3) . . ?
C29 C27 C28 110.6(3) . . ?
C32 C31 C35 107.7(3) . . ?
C32 C31 C36 128.0(3) . . ?
C35 C31 C36 124.1(3) . . ?
C32 C31 Co1 70.36(17) . . ?
C35 C31 Co1 70.20(16) . . ?
C36 C31 Co1 127.9(2) . . ?
C33 C32 C31 107.6(3) . . ?
C33 C32 C37 126.5(3) . . ?
C31 C32 C37 125.8(3) . . ?
C33 C32 Co1 69.77(17) . . ?
C31 C32 Co1 70.13(16) . . ?
C37 C32 Co1 127.1(3) . . ?
C32 C33 C34 108.8(3) . . ?
C32 C33 C38 125.3(4) . . ?
C34 C33 C38 125.9(3) . . ?
C32 C33 Co1 70.76(16) . . ?
C34 C33 Co1 70.75(16) . . ?
C38 C33 Co1 125.4(3) . . ?
C35 C34 C33 107.8(3) . . ?
C35 C34 C39 127.4(4) . . ?
C33 C34 C39 124.9(3) . . ?
C35 C34 Co1 70.43(16) . . ?
C33 C34 Co1 69.69(18) . . ?
C39 C34 Co1 124.7(2) . . ?
C34 C35 C31 108.1(3) . . ?
C34 C35 C40 127.2(3) . . ?
C31 C35 C40 124.7(3) . . ?
C34 C35 Co1 70.42(18) . . ?
C31 C35 Co1 69.89(17) . . ?
C40 C35 Co1 127.3(2) . . ?
O41 C41 Co1 132.6(2) . . ?
O41 C41 Ca1 40.59(11) . . ?
Co1 C41 Ca1 170.99(13) . . ?
C41 O41 Ca1 117.88(15) . . ?
C41 O41 Ca1 134.10(16) . 3_666 ?
Ca1 O41 Ca1 106.09(6) . 3_666 ?
O42 C42 Co1 171.6(3) . . ?
O42 C42 Ca1 46.73(17) . 3_666 ?
Co1 C42 Ca1 126.13(13) . 3_666 ?
C42 O42 Ca1 112.8(2) . 3_666 ?

_refine_diff_density_max         0.522
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.045



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-Rh
_database_code_depnum_ccdc_archive 'CCDC 2265689'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2023-05-26 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H99 Ca2 N4 O2 Rh, 1.75(C6 H14)'
_chemical_formula_sum            'C80.50 H123.50 Ca2 N4 O2 Rh'
_chemical_formula_weight         1362.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.1756(5)
_cell_length_b                   14.8989(6)
_cell_length_c                   36.7539(13)
_cell_angle_alpha                90
_cell_angle_beta                 97.759(3)
_cell_angle_gamma                90
_cell_volume                     7691.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3686
_cell_measurement_theta_min      3.6760
_cell_measurement_theta_max      69.7270

_exptl_crystal_description       blocks
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_F_000             2942
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    3.303
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            44222
_diffrn_reflns_av_unetI/netI     0.2896
_diffrn_reflns_av_R_equivalents  0.3167
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         3.205
_diffrn_reflns_theta_max         75.131
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             15187
_reflns_number_gt                4291
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0681P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00052(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         15187
_refine_ls_number_parameters     729
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2409
_refine_ls_R_factor_gt           0.0935
_refine_ls_wR_factor_ref         0.2724
_refine_ls_wR_factor_gt          0.1913
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_restrained_S_all      0.890
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.45502(5) 0.25870(5) 0.57989(2) 0.0549(3) Uani 1 1 d . . . . .
Ca1 Ca 0.48050(14) 0.17535(13) 0.66041(5) 0.0564(6) Uani 1 1 d . . . . .
Ca2 Ca 0.31311(14) 0.35316(13) 0.62986(5) 0.0571(6) Uani 1 1 d . . . . .
N1 N 0.5635(5) 0.1926(5) 0.7198(2) 0.054(2) Uani 1 1 d . . . . .
C1 C 0.5782(7) 0.1274(7) 0.7448(2) 0.058(3) Uani 1 1 d . . . . .
C2 C 0.5530(6) 0.0351(6) 0.7394(2) 0.056(3) Uani 1 1 d . . . . .
H2A H 0.553600 0.001372 0.761369 0.067 Uiso 1 1 calc R U . . .
C3 C 0.5275(6) -0.0140(7) 0.7070(3) 0.060(3) Uani 1 1 d . . . . .
N3 N 0.5075(5) 0.0221(5) 0.6731(2) 0.055(2) Uani 1 1 d . . . . .
C4 C 0.6275(7) 0.1470(6) 0.7840(2) 0.068(3) Uani 1 1 d . . . . .
H4A H 0.696161 0.136867 0.785098 0.102 Uiso 1 1 calc R U . . .
H4B H 0.601791 0.107015 0.801369 0.102 Uiso 1 1 calc R U . . .
H4C H 0.615948 0.209547 0.790312 0.102 Uiso 1 1 calc R U . . .
C5 C 0.5293(7) -0.1154(6) 0.7123(3) 0.070(3) Uani 1 1 d . . . . .
H5A H 0.491622 -0.144011 0.691110 0.105 Uiso 1 1 calc R U . . .
H5B H 0.502383 -0.130525 0.734672 0.105 Uiso 1 1 calc R U . . .
H5C H 0.595219 -0.136772 0.714390 0.105 Uiso 1 1 calc R U . . .
C6 C 0.6074(7) 0.2762(7) 0.7286(2) 0.055(3) Uani 1 1 d . . . . .
C7 C 0.7019(7) 0.2899(6) 0.7197(2) 0.056(3) Uani 1 1 d . . . . .
C8 C 0.7431(8) 0.3760(7) 0.7265(3) 0.068(3) Uani 1 1 d . . . . .
H8A H 0.804509 0.387600 0.719951 0.081 Uiso 1 1 calc R U . . .
C9 C 0.6969(8) 0.4420(7) 0.7420(3) 0.078(3) Uani 1 1 d . . . . .
H9A H 0.728085 0.497636 0.747717 0.093 Uiso 1 1 calc R U . . .
C10 C 0.6044(8) 0.4298(7) 0.7499(3) 0.075(3) Uani 1 1 d . . . . .
H10A H 0.572315 0.477655 0.760148 0.091 Uiso 1 1 calc R U . . .
C11 C 0.5585(7) 0.3472(7) 0.7427(2) 0.056(3) Uani 1 1 d . . . . .
C12 C 0.7559(7) 0.2192(7) 0.7010(3) 0.063(3) Uani 1 1 d . . . . .
H12A H 0.715339 0.164068 0.698080 0.076 Uiso 1 1 calc R U . . .
C13 C 0.7731(7) 0.2492(7) 0.6623(3) 0.082(4) Uani 1 1 d . . . . .
H13A H 0.711907 0.254094 0.646441 0.123 Uiso 1 1 calc R U . . .
H13B H 0.813185 0.204893 0.652009 0.123 Uiso 1 1 calc R U . . .
H13C H 0.805024 0.307658 0.663864 0.123 Uiso 1 1 calc R U . . .
C14 C 0.8477(7) 0.1943(7) 0.7236(3) 0.082(3) Uani 1 1 d . . . . .
H14A H 0.890210 0.246454 0.726095 0.122 Uiso 1 1 calc R U . . .
H14B H 0.877835 0.145360 0.711517 0.122 Uiso 1 1 calc R U . . .
H14C H 0.835460 0.174625 0.747949 0.122 Uiso 1 1 calc R U . . .
C15 C 0.4574(7) 0.3363(7) 0.7503(3) 0.068(3) Uani 1 1 d . . . . .
H15A H 0.432230 0.278210 0.739395 0.082 Uiso 1 1 calc R U . . .
C16 C 0.4509(8) 0.3340(7) 0.7922(3) 0.096(4) Uani 1 1 d . . . . .
H16A H 0.483176 0.386729 0.804023 0.144 Uiso 1 1 calc R U . . .
H16B H 0.481488 0.279356 0.802934 0.144 Uiso 1 1 calc R U . . .
H16C H 0.383841 0.334544 0.796153 0.144 Uiso 1 1 calc R U . . .
C17 C 0.3918(6) 0.4129(6) 0.7334(3) 0.069(3) Uani 1 1 d . . . . .
H17A H 0.326321 0.401375 0.737912 0.103 Uiso 1 1 calc R U . . .
H17B H 0.393912 0.415549 0.706853 0.103 Uiso 1 1 calc R U . . .
H17C H 0.413646 0.470165 0.744607 0.103 Uiso 1 1 calc R U . . .
C18 C 0.5042(7) -0.0378(6) 0.6416(2) 0.057(3) Uani 1 1 d . . . . .
C19 C 0.4144(8) -0.0566(6) 0.6213(3) 0.062(3) Uani 1 1 d . . . . .
C20 C 0.4147(8) -0.1078(7) 0.5892(3) 0.074(3) Uani 1 1 d . . . . .
H20A H 0.356024 -0.124711 0.575317 0.089 Uiso 1 1 calc R U . . .
C21 C 0.4990(9) -0.1339(7) 0.5777(3) 0.078(4) Uani 1 1 d . . . . .
H21A H 0.497109 -0.164902 0.555045 0.094 Uiso 1 1 calc R U . . .
C22 C 0.5848(9) -0.1168(7) 0.5978(3) 0.088(4) Uani 1 1 d . . . . .
H22A H 0.641618 -0.137845 0.589604 0.105 Uiso 1 1 calc R U . . .
C23 C 0.5890(7) -0.0688(7) 0.6299(3) 0.064(3) Uani 1 1 d . . . . .
C24 C 0.3198(7) -0.0281(7) 0.6340(3) 0.070(3) Uani 1 1 d . . . . .
H24A H 0.329508 0.032515 0.645560 0.084 Uiso 1 1 calc R U . . .
C25 C 0.2923(8) -0.0941(7) 0.6639(3) 0.095(4) Uani 1 1 d . . . . .
H25A H 0.231462 -0.075435 0.671385 0.142 Uiso 1 1 calc R U . . .
H25B H 0.341833 -0.093144 0.685211 0.142 Uiso 1 1 calc R U . . .
H25C H 0.286178 -0.154959 0.653753 0.142 Uiso 1 1 calc R U . . .
C26 C 0.2377(7) -0.0215(7) 0.6038(3) 0.095(4) Uani 1 1 d . . . . .
H26A H 0.215185 -0.081959 0.596484 0.143 Uiso 1 1 calc R U . . .
H26B H 0.258366 0.009130 0.582603 0.143 Uiso 1 1 calc R U . . .
H26C H 0.185927 0.012505 0.612411 0.143 Uiso 1 1 calc R U . . .
C27 C 0.6871(8) -0.0493(8) 0.6519(3) 0.083(4) Uani 1 1 d . . . . .
H27A H 0.676376 -0.020603 0.675620 0.100 Uiso 1 1 calc R U . . .
C28 C 0.7419(8) 0.0179(8) 0.6309(3) 0.109(5) Uani 1 1 d . . . . .
H28A H 0.803703 0.030996 0.645344 0.164 Uiso 1 1 calc R U . . .
H28B H 0.705142 0.073537 0.626803 0.164 Uiso 1 1 calc R U . . .
H28C H 0.751921 -0.007969 0.607224 0.164 Uiso 1 1 calc R U . . .
C29 C 0.7449(8) -0.1363(8) 0.6612(3) 0.115(5) Uani 1 1 d . . . . .
H29A H 0.753072 -0.167704 0.638365 0.172 Uiso 1 1 calc R U . . .
H29B H 0.710851 -0.175123 0.676496 0.172 Uiso 1 1 calc R U . . .
H29C H 0.807529 -0.121041 0.674442 0.172 Uiso 1 1 calc R U . . .
N31 N 0.1662(5) 0.3363(5) 0.65333(19) 0.053(2) Uani 1 1 d . . . . .
C31 C 0.1183(7) 0.4035(8) 0.6667(3) 0.061(3) Uani 1 1 d . . . . .
C32 C 0.1405(7) 0.4954(8) 0.6665(3) 0.075(3) Uani 1 1 d . . . . .
H32A H 0.107558 0.531977 0.681860 0.089 Uiso 1 1 calc R U . . .
C33 C 0.2065(8) 0.5427(6) 0.6463(3) 0.063(3) Uani 1 1 d . . . . .
N33 N 0.2680(6) 0.5051(5) 0.6275(2) 0.058(2) Uani 1 1 d . . . . .
C34 C 0.0234(7) 0.3830(7) 0.6800(3) 0.086(4) Uani 1 1 d . . . . .
H34A H -0.027356 0.383057 0.659090 0.130 Uiso 1 1 calc R U . . .
H34B H 0.009957 0.428823 0.697754 0.130 Uiso 1 1 calc R U . . .
H34C H 0.026519 0.323875 0.691836 0.130 Uiso 1 1 calc R U . . .
C35 C 0.1919(8) 0.6433(6) 0.6479(3) 0.083(4) Uani 1 1 d . . . . .
H35A H 0.252307 0.673932 0.646183 0.124 Uiso 1 1 calc R U . . .
H35B H 0.169387 0.659048 0.671111 0.124 Uiso 1 1 calc R U . . .
H35C H 0.144509 0.661907 0.627340 0.124 Uiso 1 1 calc R U . . .
C36 C 0.1260(7) 0.2473(7) 0.6527(3) 0.058(3) Uani 1 1 d . . . . .
C37 C 0.0595(7) 0.2248(7) 0.6220(3) 0.063(3) Uani 1 1 d . . . . .
C38 C 0.0149(7) 0.1411(7) 0.6216(3) 0.077(3) Uani 1 1 d . . . . .
H38A H -0.029383 0.124057 0.601015 0.093 Uiso 1 1 calc R U . . .
C39 C 0.0349(8) 0.0824(7) 0.6511(3) 0.083(4) Uani 1 1 d . . . . .
H39A H 0.002028 0.026893 0.651130 0.099 Uiso 1 1 calc R U . . .
C40 C 0.1013(8) 0.1046(8) 0.6797(3) 0.083(4) Uani 1 1 d . . . . .
H40A H 0.116477 0.062990 0.699188 0.100 Uiso 1 1 calc R U . . .
C41 C 0.1484(7) 0.1880(8) 0.6812(3) 0.064(3) Uani 1 1 d . . . . .
C42 C 0.0409(7) 0.2850(7) 0.5880(3) 0.071(3) Uani 1 1 d . . . . .
H42A H 0.065846 0.346261 0.595059 0.085 Uiso 1 1 calc R U . . .
C43 C 0.0962(8) 0.2488(7) 0.5580(3) 0.098(4) Uani 1 1 d . . . . .
H43A H 0.164652 0.252378 0.566478 0.146 Uiso 1 1 calc R U . . .
H43B H 0.080909 0.284876 0.535695 0.146 Uiso 1 1 calc R U . . .
H43C H 0.078240 0.186197 0.552724 0.146 Uiso 1 1 calc R U . . .
C44 C -0.0660(7) 0.2936(8) 0.5740(3) 0.108(4) Uani 1 1 d . . . . .
H44A H -0.088362 0.238710 0.560928 0.162 Uiso 1 1 calc R U . . .
H44B H -0.076494 0.345042 0.557376 0.162 Uiso 1 1 calc R U . . .
H44C H -0.101302 0.302521 0.594929 0.162 Uiso 1 1 calc R U . . .
C45 C 0.2240(7) 0.2109(7) 0.7134(3) 0.066(3) Uani 1 1 d . . . . .
H45A H 0.264707 0.259415 0.705054 0.080 Uiso 1 1 calc R U . . .
C46 C 0.1806(8) 0.2476(7) 0.7468(3) 0.098(4) Uani 1 1 d . . . . .
H46A H 0.135871 0.203582 0.754493 0.147 Uiso 1 1 calc R U . . .
H46B H 0.146971 0.303865 0.740059 0.147 Uiso 1 1 calc R U . . .
H46C H 0.231612 0.258665 0.767135 0.147 Uiso 1 1 calc R U . . .
C47 C 0.2907(7) 0.1284(7) 0.7250(3) 0.087(4) Uani 1 1 d . . . . .
H47A H 0.345345 0.148275 0.742298 0.130 Uiso 1 1 calc R U . . .
H47B H 0.313215 0.102855 0.703127 0.130 Uiso 1 1 calc R U . . .
H47C H 0.255083 0.082769 0.736652 0.130 Uiso 1 1 calc R U . . .
C48 C 0.3119(8) 0.5595(6) 0.6028(3) 0.061(3) Uani 1 1 d . . . . .
C49 C 0.4066(9) 0.5840(6) 0.6124(3) 0.067(3) Uani 1 1 d . . . . .
C50 C 0.4513(9) 0.6295(7) 0.5864(3) 0.086(4) Uani 1 1 d . . . . .
H50A H 0.516135 0.646578 0.592162 0.103 Uiso 1 1 calc R U . . .
C51 C 0.4021(11) 0.6505(8) 0.5518(3) 0.095(4) Uani 1 1 d . . . . .
H51A H 0.433091 0.682505 0.534486 0.114 Uiso 1 1 calc R U . . .
C52 C 0.3067(10) 0.6242(8) 0.5429(3) 0.092(4) Uani 1 1 d . . . . .
H52A H 0.273513 0.636980 0.519246 0.110 Uiso 1 1 calc R U . . .
C53 C 0.2617(9) 0.5801(7) 0.5683(3) 0.067(3) Uani 1 1 d . . . . .
C54 C 0.4622(8) 0.5694(7) 0.6501(3) 0.074(3) Uani 1 1 d . . . . .
H54A H 0.438907 0.511858 0.659721 0.089 Uiso 1 1 calc R U . . .
C55 C 0.4467(9) 0.6412(9) 0.6775(3) 0.136(6) Uani 1 1 d . . . . .
H55A H 0.485174 0.627975 0.701062 0.204 Uiso 1 1 calc R U . . .
H55B H 0.379228 0.642960 0.680723 0.204 Uiso 1 1 calc R U . . .
H55C H 0.465562 0.699548 0.668451 0.204 Uiso 1 1 calc R U . . .
C56 C 0.5697(8) 0.5594(7) 0.6505(3) 0.101(4) Uani 1 1 d . . . . .
H56A H 0.598908 0.618980 0.650401 0.152 Uiso 1 1 calc R U . . .
H56B H 0.582274 0.525895 0.628758 0.152 Uiso 1 1 calc R U . . .
H56C H 0.596684 0.526915 0.672698 0.152 Uiso 1 1 calc R U . . .
C57 C 0.1554(8) 0.5561(8) 0.5582(3) 0.083(3) Uani 1 1 d . . . . .
H57A H 0.130317 0.535174 0.580956 0.099 Uiso 1 1 calc R U . . .
C58 C 0.1447(8) 0.4806(8) 0.5304(4) 0.135(6) Uani 1 1 d . . . . .
H58A H 0.169223 0.500017 0.508040 0.202 Uiso 1 1 calc R U . . .
H58B H 0.077264 0.464692 0.524601 0.202 Uiso 1 1 calc R U . . .
H58C H 0.180672 0.428158 0.540702 0.202 Uiso 1 1 calc R U . . .
C59 C 0.0951(10) 0.6360(8) 0.5423(3) 0.137(6) Uani 1 1 d . . . . .
H59A H 0.108766 0.648386 0.517348 0.206 Uiso 1 1 calc R U . . .
H59B H 0.110564 0.688926 0.557757 0.206 Uiso 1 1 calc R U . . .
H59C H 0.027386 0.621585 0.541582 0.206 Uiso 1 1 calc R U . . .
C63 C 0.4306(5) 0.3054(5) 0.52074(19) 0.066(3) Uani 1 1 d G . . . .
C62 C 0.4303(4) 0.2101(5) 0.52059(18) 0.072(3) Uani 1 1 d G . . . .
C61 C 0.5218(6) 0.1803(4) 0.53646(19) 0.062(3) Uani 1 1 d G . . . .
C65 C 0.5787(4) 0.2571(6) 0.54641(17) 0.064(3) Uani 1 1 d G . . . .
C64 C 0.5223(6) 0.3345(4) 0.53670(19) 0.067(3) Uani 1 1 d G . . . .
C66 C 0.5545(8) 0.0823(7) 0.5389(3) 0.091(4) Uani 1 1 d . . . . .
H66A H 0.610718 0.076708 0.557440 0.136 Uiso 1 1 calc R U . . .
H66B H 0.570524 0.062965 0.514987 0.136 Uiso 1 1 calc R U . . .
H66C H 0.503159 0.044564 0.545794 0.136 Uiso 1 1 calc R U . . .
C67 C 0.3494(7) 0.1504(7) 0.5050(3) 0.092(4) Uani 1 1 d . . . . .
H67A H 0.341989 0.101779 0.522411 0.138 Uiso 1 1 calc R U . . .
H67B H 0.362916 0.124814 0.481730 0.138 Uiso 1 1 calc R U . . .
H67C H 0.290536 0.185554 0.500864 0.138 Uiso 1 1 calc R U . . .
C68 C 0.3525(7) 0.3678(7) 0.5035(3) 0.095(4) Uani 1 1 d . . . . .
H68A H 0.290446 0.344475 0.507911 0.142 Uiso 1 1 calc R U . . .
H68B H 0.354560 0.371712 0.476991 0.142 Uiso 1 1 calc R U . . .
H68C H 0.362125 0.427684 0.514435 0.142 Uiso 1 1 calc R U . . .
C69 C 0.5612(8) 0.4298(6) 0.5409(3) 0.084(4) Uani 1 1 d . . . . .
H69A H 0.508170 0.472190 0.540503 0.126 Uiso 1 1 calc R U . . .
H69B H 0.597239 0.443358 0.520633 0.126 Uiso 1 1 calc R U . . .
H69C H 0.603082 0.435190 0.564295 0.126 Uiso 1 1 calc R U . . .
C70 C 0.6842(6) 0.2562(6) 0.5601(3) 0.073(3) Uani 1 1 d . . . . .
H70A H 0.700751 0.200148 0.573414 0.110 Uiso 1 1 calc R U . . .
H70B H 0.700140 0.307267 0.576591 0.110 Uiso 1 1 calc R U . . .
H70C H 0.720121 0.260524 0.539180 0.110 Uiso 1 1 calc R U . . .
C71 C 0.3559(6) 0.1950(6) 0.5992(3) 0.057(3) Uani 1 1 d . . . . .
H71A H 0.321628 0.155728 0.581790 0.069 Uiso 1 1 calc R U . . .
O71 O 0.3252(4) 0.1937(4) 0.63072(16) 0.0564(17) Uani 1 1 d . . . . .
C72 C 0.4988(6) 0.3276(6) 0.6234(2) 0.056(3) Uani 1 1 d . . . . .
H72A H 0.551046 0.365759 0.620644 0.067 Uiso 1 1 calc R U . . .
O72 O 0.4716(4) 0.3324(4) 0.65528(16) 0.0514(16) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C71 1.910(8) . ?
Rh1 C72 1.930(9) . ?
Rh1 C64 2.261(6) . ?
Rh1 C63 2.264(6) . ?
Rh1 C65 2.274(6) . ?
Rh1 C62 2.279(6) . ?
Rh1 C61 2.285(6) . ?
Rh1 Ca1 3.1847(19) . ?
Rh1 Ca2 3.225(2) . ?
Ca1 O71 2.337(6) . ?
Ca1 O72 2.350(6) . ?
Ca1 N1 2.351(7) . ?
Ca1 N3 2.351(7) . ?
Ca2 O72 2.334(6) . ?
Ca2 N33 2.351(8) . ?
Ca2 N31 2.372(8) . ?
Ca2 O71 2.382(6) . ?
N1 C1 1.333(10) . ?
N1 C6 1.410(11) . ?
C1 C2 1.429(12) . ?
C1 C4 1.541(11) . ?
C2 C3 1.402(11) . ?
C3 N3 1.353(10) . ?
C3 C5 1.521(11) . ?
N3 C18 1.458(10) . ?
C6 C11 1.402(12) . ?
C6 C7 1.436(12) . ?
C7 C8 1.418(12) . ?
C7 C12 1.519(12) . ?
C8 C9 1.349(12) . ?
C9 C10 1.393(13) . ?
C10 C11 1.401(12) . ?
C11 C15 1.506(12) . ?
C12 C14 1.494(12) . ?
C12 C13 1.540(11) . ?
C15 C17 1.548(11) . ?
C15 C16 1.555(12) . ?
C18 C23 1.407(12) . ?
C18 C19 1.413(12) . ?
C19 C20 1.404(12) . ?
C19 C24 1.537(13) . ?
C20 C21 1.376(14) . ?
C21 C22 1.358(14) . ?
C22 C23 1.377(12) . ?
C23 C27 1.539(13) . ?
C24 C26 1.501(12) . ?
C24 C25 1.561(12) . ?
C27 C28 1.538(13) . ?
C27 C29 1.546(13) . ?
N31 C31 1.340(11) . ?
N31 C36 1.442(11) . ?
C31 C32 1.406(13) . ?
C31 C34 1.524(12) . ?
C32 C33 1.454(13) . ?
C33 N33 1.309(11) . ?
C33 C35 1.515(12) . ?
N33 C48 1.421(11) . ?
C36 C41 1.375(12) . ?
C36 C37 1.409(12) . ?
C37 C38 1.398(12) . ?
C37 C42 1.529(12) . ?
C38 C39 1.391(13) . ?
C39 C40 1.354(13) . ?
C40 C41 1.407(13) . ?
C41 C45 1.525(12) . ?
C42 C43 1.535(12) . ?
C42 C44 1.538(12) . ?
C45 C46 1.545(12) . ?
C45 C47 1.573(12) . ?
C48 C49 1.390(13) . ?
C48 C53 1.402(13) . ?
C49 C50 1.393(12) . ?
C49 C54 1.515(13) . ?
C50 C51 1.399(14) . ?
C51 C52 1.403(15) . ?
C52 C53 1.367(13) . ?
C53 C57 1.545(14) . ?
C54 C55 1.504(13) . ?
C54 C56 1.528(13) . ?
C57 C58 1.513(13) . ?
C57 C59 1.535(13) . ?
C63 C64 1.4200 . ?
C63 C62 1.4200 . ?
C63 C68 1.518(10) . ?
C62 C61 1.4200 . ?
C62 C67 1.502(10) . ?
C61 C65 1.4200 . ?
C61 C66 1.530(10) . ?
C65 C64 1.4200 . ?
C65 C70 1.512(10) . ?
C64 C69 1.524(10) . ?
C71 O71 1.292(9) . ?
C72 O72 1.285(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C71 Rh1 C72 97.3(4) . . ?
C71 Rh1 C64 155.5(3) . . ?
C72 Rh1 C64 101.4(3) . . ?
C71 Rh1 C63 119.0(3) . . ?
C72 Rh1 C63 128.5(4) . . ?
C64 Rh1 C63 36.57(9) . . ?
C71 Rh1 C65 148.8(4) . . ?
C72 Rh1 C65 105.6(3) . . ?
C64 Rh1 C65 36.49(9) . . ?
C63 Rh1 C65 60.83(10) . . ?
C71 Rh1 C62 99.9(3) . . ?
C72 Rh1 C62 162.2(3) . . ?
C64 Rh1 C62 60.80(11) . . ?
C63 Rh1 C62 36.43(9) . . ?
C65 Rh1 C62 60.62(10) . . ?
C71 Rh1 C61 113.6(3) . . ?
C72 Rh1 C61 137.2(3) . . ?
C64 Rh1 C61 60.71(10) . . ?
C63 Rh1 C61 60.67(11) . . ?
C65 Rh1 C61 36.29(9) . . ?
C62 Rh1 C61 36.26(9) . . ?
C71 Rh1 Ca1 57.2(3) . . ?
C72 Rh1 Ca1 56.9(3) . . ?
C64 Rh1 Ca1 147.3(2) . . ?
C63 Rh1 Ca1 174.5(2) . . ?
C65 Rh1 Ca1 119.99(16) . . ?
C62 Rh1 Ca1 138.4(2) . . ?
C61 Rh1 Ca1 116.37(16) . . ?
C71 Rh1 Ca2 57.2(3) . . ?
C72 Rh1 Ca2 56.7(3) . . ?
C64 Rh1 Ca2 122.47(18) . . ?
C63 Rh1 Ca2 112.75(16) . . ?
C65 Rh1 Ca2 154.0(2) . . ?
C62 Rh1 Ca2 131.03(19) . . ?
C61 Rh1 Ca2 166.1(2) . . ?
Ca1 Rh1 Ca2 69.03(5) . . ?
O71 Ca1 O72 79.0(2) . . ?
O71 Ca1 N1 138.0(3) . . ?
O72 Ca1 N1 88.9(2) . . ?
O71 Ca1 N3 108.9(2) . . ?
O72 Ca1 N3 171.3(2) . . ?
N1 Ca1 N3 82.8(3) . . ?
O72 Ca2 N33 112.6(2) . . ?
O72 Ca2 N31 133.2(2) . . ?
N33 Ca2 N31 82.4(3) . . ?
O72 Ca2 O71 78.4(2) . . ?
N33 Ca2 O71 168.5(3) . . ?
N31 Ca2 O71 87.4(2) . . ?
C1 N1 C6 117.6(8) . . ?
C1 N1 Ca1 124.9(6) . . ?
C6 N1 Ca1 117.3(6) . . ?
N1 C1 C2 126.4(9) . . ?
N1 C1 C4 120.9(9) . . ?
C2 C1 C4 112.7(8) . . ?
C3 C2 C1 130.6(9) . . ?
N3 C3 C2 124.9(9) . . ?
N3 C3 C5 120.6(9) . . ?
C2 C3 C5 114.3(8) . . ?
C3 N3 C18 118.0(8) . . ?
C3 N3 Ca1 125.2(6) . . ?
C18 N3 Ca1 116.8(5) . . ?
C11 C6 N1 121.7(9) . . ?
C11 C6 C7 120.1(9) . . ?
N1 C6 C7 118.0(9) . . ?
C8 C7 C6 117.5(10) . . ?
C8 C7 C12 119.2(9) . . ?
C6 C7 C12 123.2(9) . . ?
C9 C8 C7 121.5(11) . . ?
C8 C9 C10 121.2(11) . . ?
C9 C10 C11 120.1(10) . . ?
C10 C11 C6 119.5(10) . . ?
C10 C11 C15 119.2(10) . . ?
C6 C11 C15 121.3(9) . . ?
C14 C12 C7 112.1(8) . . ?
C14 C12 C13 110.5(8) . . ?
C7 C12 C13 111.6(8) . . ?
C11 C15 C17 112.3(9) . . ?
C11 C15 C16 111.9(8) . . ?
C17 C15 C16 107.6(8) . . ?
C23 C18 C19 121.4(9) . . ?
C23 C18 N3 120.3(9) . . ?
C19 C18 N3 118.0(9) . . ?
C20 C19 C18 116.4(10) . . ?
C20 C19 C24 120.5(9) . . ?
C18 C19 C24 123.0(9) . . ?
C21 C20 C19 120.9(10) . . ?
C22 C21 C20 122.1(11) . . ?
C21 C22 C23 119.7(12) . . ?
C22 C23 C18 119.4(10) . . ?
C22 C23 C27 118.7(10) . . ?
C18 C23 C27 121.9(10) . . ?
C26 C24 C19 114.4(9) . . ?
C26 C24 C25 108.6(9) . . ?
C19 C24 C25 110.6(9) . . ?
C28 C27 C23 110.0(9) . . ?
C28 C27 C29 111.5(10) . . ?
C23 C27 C29 111.8(10) . . ?
C31 N31 C36 118.3(8) . . ?
C31 N31 Ca2 124.6(7) . . ?
C36 N31 Ca2 117.1(6) . . ?
N31 C31 C32 127.0(10) . . ?
N31 C31 C34 118.8(10) . . ?
C32 C31 C34 113.8(10) . . ?
C31 C32 C33 129.3(10) . . ?
N33 C33 C32 125.7(9) . . ?
N33 C33 C35 123.2(10) . . ?
C32 C33 C35 111.0(10) . . ?
C33 N33 C48 118.3(8) . . ?
C33 N33 Ca2 126.1(7) . . ?
C48 N33 Ca2 115.6(6) . . ?
C41 C36 C37 121.2(10) . . ?
C41 C36 N31 121.9(9) . . ?
C37 C36 N31 116.9(9) . . ?
C38 C37 C36 118.2(10) . . ?
C38 C37 C42 119.2(10) . . ?
C36 C37 C42 122.4(9) . . ?
C39 C38 C37 120.6(10) . . ?
C40 C39 C38 119.9(11) . . ?
C39 C40 C41 121.4(11) . . ?
C36 C41 C40 118.6(10) . . ?
C36 C41 C45 121.0(10) . . ?
C40 C41 C45 120.4(10) . . ?
C37 C42 C43 109.4(9) . . ?
C37 C42 C44 112.0(9) . . ?
C43 C42 C44 111.4(8) . . ?
C41 C45 C46 112.6(9) . . ?
C41 C45 C47 111.6(9) . . ?
C46 C45 C47 110.6(8) . . ?
C49 C48 C53 121.8(10) . . ?
C49 C48 N33 118.5(10) . . ?
C53 C48 N33 119.4(10) . . ?
C49 C48 Ca2 102.0(7) . . ?
C53 C48 Ca2 117.9(7) . . ?
N33 C48 Ca2 41.0(4) . . ?
C48 C49 C50 117.8(11) . . ?
C48 C49 C54 124.1(9) . . ?
C50 C49 C54 118.0(11) . . ?
C49 C50 C51 121.0(12) . . ?
C50 C51 C52 119.8(12) . . ?
C53 C52 C51 119.9(12) . . ?
C52 C53 C48 119.7(12) . . ?
C52 C53 C57 118.6(11) . . ?
C48 C53 C57 121.6(10) . . ?
C55 C54 C49 113.8(9) . . ?
C55 C54 C56 107.4(9) . . ?
C49 C54 C56 114.7(10) . . ?
C58 C57 C59 108.6(9) . . ?
C58 C57 C53 109.8(10) . . ?
C59 C57 C53 112.7(11) . . ?
C64 C63 C62 108.0 . . ?
C64 C63 C68 124.1(8) . . ?
C62 C63 C68 127.6(8) . . ?
C64 C63 Rh1 71.6(3) . . ?
C62 C63 Rh1 72.3(3) . . ?
C68 C63 Rh1 126.7(5) . . ?
C61 C62 C63 108.0 . . ?
C61 C62 C67 125.4(7) . . ?
C63 C62 C67 126.5(7) . . ?
C61 C62 Rh1 72.1(3) . . ?
C63 C62 Rh1 71.2(3) . . ?
C67 C62 Rh1 124.3(6) . . ?
C62 C61 C65 108.0 . . ?
C62 C61 C66 125.1(7) . . ?
C65 C61 C66 126.7(7) . . ?
C62 C61 Rh1 71.6(3) . . ?
C65 C61 Rh1 71.4(3) . . ?
C66 C61 Rh1 126.7(6) . . ?
C64 C65 C61 108.0 . . ?
C64 C65 C70 126.1(7) . . ?
C61 C65 C70 125.4(7) . . ?
C64 C65 Rh1 71.3(3) . . ?
C61 C65 Rh1 72.3(3) . . ?
C70 C65 Rh1 128.3(5) . . ?
C63 C64 C65 108.0 . . ?
C63 C64 C69 128.7(7) . . ?
C65 C64 C69 123.2(7) . . ?
C63 C64 Rh1 71.8(3) . . ?
C65 C64 Rh1 72.2(3) . . ?
C69 C64 Rh1 125.1(6) . . ?
O71 C71 Rh1 133.9(7) . . ?
O71 C71 Ca1 60.6(4) . . ?
Rh1 C71 Ca1 86.1(3) . . ?
O71 C71 Ca2 61.3(5) . . ?
Rh1 C71 Ca2 86.5(3) . . ?
Ca1 C71 Ca2 84.5(3) . . ?
C71 O71 Ca1 90.7(5) . . ?
C71 O71 Ca2 90.3(5) . . ?
Ca1 O71 Ca2 100.6(2) . . ?
O72 C72 Rh1 133.1(7) . . ?
O72 C72 Ca1 61.4(5) . . ?
Rh1 C72 Ca1 85.9(3) . . ?
O72 C72 Ca2 59.7(4) . . ?
Rh1 C72 Ca2 86.6(3) . . ?
Ca1 C72 Ca2 85.0(3) . . ?
C72 O72 Ca2 91.9(5) . . ?
C72 O72 Ca1 89.9(5) . . ?
Ca2 O72 Ca1 101.7(2) . . ?

_refine_diff_density_max         0.781
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.097



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-Ir
_database_code_depnum_ccdc_archive 'CCDC 2265690'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2023-05-26 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H99 Ca2 Ir N4 O2, 1.5(C6 H14)'
_chemical_formula_sum            'C79 H120 Ca2 Ir N4 O2'
_chemical_formula_weight         1430.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.2170(3)
_cell_length_b                   14.8985(3)
_cell_length_c                   36.7785(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.7586(15)
_cell_angle_gamma                90
_cell_volume                     7718.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5741
_cell_measurement_theta_min      4.2940
_cell_measurement_theta_max      73.3690

_exptl_crystal_description       'platy needles'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_F_000             3020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.046
_exptl_absorpt_coefficient_mu    4.844
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            24904
_diffrn_reflns_av_unetI/netI     0.0985
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         3.833
_diffrn_reflns_theta_max         73.472
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measured_fraction_theta_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             14472
_reflns_number_gt                8974
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          Twin,SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0844P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14472
_refine_ls_number_parameters     728
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1684
_refine_ls_wR_factor_gt          0.1539
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_restrained_S_all      0.960
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.45441(2) 0.25894(2) 0.58007(2) 0.03749(10) Uani 1 1 d . . . . .
Ca1 Ca 0.47947(12) 0.17533(9) 0.66078(4) 0.0385(3) Uani 1 1 d . . . . .
Ca2 Ca 0.31282(11) 0.35247(10) 0.63018(4) 0.0396(3) Uani 1 1 d . . . . .
N1 N 0.5650(4) 0.1914(4) 0.72020(16) 0.0374(13) Uani 1 1 d . . . . .
C1 C 0.5783(5) 0.1271(5) 0.74519(18) 0.0379(16) Uani 1 1 d . . . . .
C2 C 0.5516(6) 0.0351(5) 0.7391(2) 0.0420(17) Uani 1 1 d . . . . .
H2A H 0.550018 0.001046 0.760827 0.050 Uiso 1 1 calc R U . . .
C3 C 0.5273(6) -0.0132(5) 0.7064(2) 0.0415(16) Uani 1 1 d . . . . .
N3 N 0.5081(4) 0.0208(4) 0.67337(16) 0.0378(13) Uani 1 1 d . . . . .
C4 C 0.6266(8) 0.1472(6) 0.7837(2) 0.060(2) Uani 1 1 d . . . . .
H4A H 0.694063 0.131777 0.785524 0.090 Uiso 1 1 calc R U . . .
H4B H 0.596842 0.111599 0.801425 0.090 Uiso 1 1 calc R U . . .
H4C H 0.619978 0.211194 0.788953 0.090 Uiso 1 1 calc R U . . .
C5 C 0.5310(7) -0.1143(5) 0.7122(2) 0.056(2) Uani 1 1 d . . . . .
H5A H 0.483655 -0.143167 0.694058 0.083 Uiso 1 1 calc R U . . .
H5B H 0.517204 -0.128295 0.736942 0.083 Uiso 1 1 calc R U . . .
H5C H 0.594367 -0.136455 0.709206 0.083 Uiso 1 1 calc R U . . .
C6 C 0.6082(5) 0.2768(5) 0.72843(19) 0.0410(16) Uani 1 1 d . . . . .
C7 C 0.7005(6) 0.2918(5) 0.7195(2) 0.0428(17) Uani 1 1 d . . . . .
C8 C 0.7421(6) 0.3757(6) 0.7268(2) 0.052(2) Uani 1 1 d . . . . .
H8A H 0.804084 0.386928 0.720918 0.062 Uiso 1 1 calc R U . . .
C9 C 0.6939(7) 0.4428(6) 0.7425(3) 0.061(2) Uani 1 1 d . . . . .
H9A H 0.724194 0.498780 0.748298 0.073 Uiso 1 1 calc R U . . .
C10 C 0.6052(7) 0.4298(6) 0.7497(2) 0.056(2) Uani 1 1 d . . . . .
H10A H 0.573508 0.478037 0.759740 0.067 Uiso 1 1 calc R U . . .
C11 C 0.5566(6) 0.3479(5) 0.7429(2) 0.0441(18) Uani 1 1 d . . . . .
C12 C 0.7548(6) 0.2196(6) 0.7015(2) 0.0503(19) Uani 1 1 d . . . . .
H12A H 0.714089 0.164628 0.698859 0.060 Uiso 1 1 calc R U . . .
C13 C 0.7712(7) 0.2493(8) 0.6627(3) 0.072(3) Uani 1 1 d . . . . .
H13A H 0.709789 0.259017 0.647593 0.109 Uiso 1 1 calc R U . . .
H13B H 0.806321 0.202447 0.651545 0.109 Uiso 1 1 calc R U . . .
H13C H 0.807793 0.305188 0.664305 0.109 Uiso 1 1 calc R U . . .
C14 C 0.8490(7) 0.1939(7) 0.7245(3) 0.066(3) Uani 1 1 d . . . . .
H14A H 0.891288 0.246159 0.727063 0.100 Uiso 1 1 calc R U . . .
H14B H 0.878889 0.145183 0.712357 0.100 Uiso 1 1 calc R U . . .
H14C H 0.837048 0.174050 0.748900 0.100 Uiso 1 1 calc R U . . .
C15 C 0.4565(6) 0.3372(6) 0.7505(2) 0.052(2) Uani 1 1 d . . . . .
H15A H 0.431970 0.278996 0.739543 0.063 Uiso 1 1 calc R U . . .
C16 C 0.4515(8) 0.3329(8) 0.7917(3) 0.074(3) Uani 1 1 d . . . . .
H16A H 0.484168 0.385081 0.803806 0.112 Uiso 1 1 calc R U . . .
H16B H 0.482265 0.277779 0.801844 0.112 Uiso 1 1 calc R U . . .
H16C H 0.384949 0.333168 0.796003 0.112 Uiso 1 1 calc R U . . .
C17 C 0.3923(7) 0.4110(7) 0.7334(3) 0.066(3) Uani 1 1 d . . . . .
H17A H 0.327545 0.400795 0.738922 0.099 Uiso 1 1 calc R U . . .
H17B H 0.392364 0.410917 0.706805 0.099 Uiso 1 1 calc R U . . .
H17C H 0.415242 0.469078 0.743517 0.099 Uiso 1 1 calc R U . . .
C18 C 0.5043(6) -0.0362(5) 0.6421(2) 0.0439(18) Uani 1 1 d . . . . .
C19 C 0.4148(7) -0.0578(5) 0.6219(2) 0.051(2) Uani 1 1 d . . . . .
C20 C 0.4145(9) -0.1092(6) 0.5900(3) 0.068(3) Uani 1 1 d . . . . .
H20A H 0.355704 -0.125646 0.576157 0.082 Uiso 1 1 calc R U . . .
C21 C 0.5004(9) -0.1369(7) 0.5780(3) 0.073(3) Uani 1 1 d . . . . .
H21A H 0.499022 -0.168983 0.555648 0.088 Uiso 1 1 calc R U . . .
C22 C 0.5838(8) -0.1180(6) 0.5982(2) 0.064(3) Uani 1 1 d . . . . .
H22A H 0.640987 -0.138920 0.590395 0.077 Uiso 1 1 calc R U . . .
C23 C 0.5879(7) -0.0675(6) 0.6309(2) 0.052(2) Uani 1 1 d . . . . .
C24 C 0.3217(7) -0.0306(6) 0.6349(3) 0.059(2) Uani 1 1 d . . . . .
H24A H 0.332079 0.030069 0.646333 0.070 Uiso 1 1 calc R U . . .
C25 C 0.2949(8) -0.0924(8) 0.6642(3) 0.078(3) Uani 1 1 d . . . . .
H25A H 0.234663 -0.072577 0.671688 0.117 Uiso 1 1 calc R U . . .
H25B H 0.344609 -0.091029 0.685432 0.117 Uiso 1 1 calc R U . . .
H25C H 0.288015 -0.153675 0.654559 0.117 Uiso 1 1 calc R U . . .
C26 C 0.2409(8) -0.0214(8) 0.6039(3) 0.085(4) Uani 1 1 d . . . . .
H26A H 0.215182 -0.080948 0.596953 0.128 Uiso 1 1 calc R U . . .
H26B H 0.264279 0.006607 0.582729 0.128 Uiso 1 1 calc R U . . .
H26C H 0.190925 0.016053 0.611906 0.128 Uiso 1 1 calc R U . . .
C27 C 0.6858(7) -0.0489(7) 0.6520(3) 0.062(2) Uani 1 1 d . . . . .
H27A H 0.676076 -0.020002 0.675708 0.074 Uiso 1 1 calc R U . . .
C28 C 0.7405(8) 0.0187(9) 0.6308(3) 0.086(4) Uani 1 1 d . . . . .
H28A H 0.803948 0.028437 0.644292 0.130 Uiso 1 1 calc R U . . .
H28B H 0.706004 0.075756 0.628290 0.130 Uiso 1 1 calc R U . . .
H28C H 0.746243 -0.005363 0.606390 0.130 Uiso 1 1 calc R U . . .
C29 C 0.7433(9) -0.1359(9) 0.6613(3) 0.093(4) Uani 1 1 d . . . . .
H29A H 0.752520 -0.166925 0.638567 0.140 Uiso 1 1 calc R U . . .
H29B H 0.708538 -0.175110 0.676254 0.140 Uiso 1 1 calc R U . . .
H29C H 0.805184 -0.120805 0.675041 0.140 Uiso 1 1 calc R U . . .
N31 N 0.1663(5) 0.3369(4) 0.65332(16) 0.0425(14) Uani 1 1 d . . . . .
C31 C 0.1184(6) 0.4037(6) 0.6662(2) 0.0478(19) Uani 1 1 d . . . . .
C32 C 0.1411(6) 0.4945(6) 0.6663(2) 0.050(2) Uani 1 1 d . . . . .
H32A H 0.109183 0.530171 0.682226 0.060 Uiso 1 1 calc R U . . .
C33 C 0.2035(6) 0.5426(5) 0.6468(2) 0.0450(18) Uani 1 1 d . . . . .
N33 N 0.2666(5) 0.5048(4) 0.62800(17) 0.0426(14) Uani 1 1 d . . . . .
C34 C 0.0241(7) 0.3828(7) 0.6807(3) 0.066(3) Uani 1 1 d . . . . .
H34A H -0.027394 0.380788 0.660095 0.099 Uiso 1 1 calc R U . . .
H34B H 0.010787 0.429805 0.697937 0.099 Uiso 1 1 calc R U . . .
H34C H 0.028872 0.324679 0.693236 0.099 Uiso 1 1 calc R U . . .
C35 C 0.1913(8) 0.6448(6) 0.6472(3) 0.061(2) Uani 1 1 d . . . . .
H35A H 0.243891 0.673283 0.636910 0.092 Uiso 1 1 calc R U . . .
H35B H 0.191105 0.665229 0.672547 0.092 Uiso 1 1 calc R U . . .
H35C H 0.131085 0.661108 0.632509 0.092 Uiso 1 1 calc R U . . .
C36 C 0.1242(5) 0.2494(6) 0.6527(2) 0.0477(17) Uani 1 1 d . . . . .
C37 C 0.0585(6) 0.2232(6) 0.6222(2) 0.052(2) Uani 1 1 d . . . . .
C38 C 0.0141(7) 0.1401(7) 0.6221(3) 0.063(2) Uani 1 1 d . . . . .
H38A H -0.030859 0.123318 0.601684 0.076 Uiso 1 1 calc R U . . .
C39 C 0.0344(8) 0.0823(7) 0.6509(3) 0.075(3) Uani 1 1 d . . . . .
H39A H 0.002476 0.026255 0.650826 0.089 Uiso 1 1 calc R U . . .
C40 C 0.1015(7) 0.1055(7) 0.6804(3) 0.062(2) Uani 1 1 d . . . . .
H40A H 0.115346 0.064983 0.700392 0.074 Uiso 1 1 calc R U . . .
C41 C 0.1488(6) 0.1873(6) 0.6811(2) 0.053(2) Uani 1 1 d . . . . .
C42 C 0.0402(7) 0.2815(7) 0.5884(2) 0.062(2) Uani 1 1 d . . . . .
H42A H 0.064294 0.343029 0.595481 0.074 Uiso 1 1 calc R U . . .
C43 C 0.0925(8) 0.2492(9) 0.5575(3) 0.080(3) Uani 1 1 d . . . . .
H43A H 0.160864 0.247926 0.565988 0.120 Uiso 1 1 calc R U . . .
H43B H 0.079654 0.290116 0.536576 0.120 Uiso 1 1 calc R U . . .
H43C H 0.070719 0.188721 0.550058 0.120 Uiso 1 1 calc R U . . .
C44 C -0.0658(7) 0.2905(9) 0.5733(3) 0.086(4) Uani 1 1 d . . . . .
H44A H -0.089771 0.232546 0.563335 0.128 Uiso 1 1 calc R U . . .
H44B H -0.073574 0.335694 0.553741 0.128 Uiso 1 1 calc R U . . .
H44C H -0.101407 0.308807 0.593045 0.128 Uiso 1 1 calc R U . . .
C45 C 0.2266(6) 0.2109(6) 0.7134(2) 0.052(2) Uani 1 1 d . . . . .
H45A H 0.267598 0.259107 0.704996 0.063 Uiso 1 1 calc R U . . .
C46 C 0.1840(9) 0.2464(10) 0.7461(3) 0.099(4) Uani 1 1 d . . . . .
H46A H 0.130280 0.208475 0.750457 0.149 Uiso 1 1 calc R U . . .
H46B H 0.161904 0.308055 0.741178 0.149 Uiso 1 1 calc R U . . .
H46C H 0.232128 0.245569 0.767847 0.149 Uiso 1 1 calc R U . . .
C47 C 0.2894(7) 0.1297(7) 0.7247(3) 0.071(3) Uani 1 1 d . . . . .
H47A H 0.349551 0.149901 0.738398 0.106 Uiso 1 1 calc R U . . .
H47B H 0.301877 0.097118 0.702702 0.106 Uiso 1 1 calc R U . . .
H47C H 0.256920 0.089918 0.740210 0.106 Uiso 1 1 calc R U . . .
C48 C 0.3097(7) 0.5590(5) 0.6028(2) 0.050(2) Uani 1 1 d . . . . .
C49 C 0.4061(8) 0.5851(5) 0.6121(2) 0.056(2) Uani 1 1 d . . . . .
C50 C 0.4478(9) 0.6317(6) 0.5858(3) 0.073(3) Uani 1 1 d . . . . .
H50A H 0.511939 0.650595 0.591400 0.087 Uiso 1 1 calc R U . . .
C51 C 0.3979(11) 0.6518(8) 0.5510(3) 0.091(4) Uani 1 1 d . . . . .
H51A H 0.428060 0.683437 0.533356 0.110 Uiso 1 1 calc R U . . .
C52 C 0.3064(10) 0.6256(7) 0.5431(3) 0.082(4) Uani 1 1 d . . . . .
H52A H 0.272653 0.638436 0.519615 0.098 Uiso 1 1 calc R U . . .
C53 C 0.2612(8) 0.5808(6) 0.5683(2) 0.060(2) Uani 1 1 d . . . . .
C54 C 0.4623(7) 0.5671(6) 0.6497(3) 0.063(2) Uani 1 1 d . . . . .
H54A H 0.439587 0.508155 0.658145 0.075 Uiso 1 1 calc R U . . .
C55 C 0.4413(10) 0.6353(10) 0.6772(3) 0.107(5) Uani 1 1 d . . . . .
H55A H 0.476498 0.620363 0.701248 0.161 Uiso 1 1 calc R U . . .
H55B H 0.373123 0.635463 0.678877 0.161 Uiso 1 1 calc R U . . .
H55C H 0.460691 0.694813 0.669648 0.161 Uiso 1 1 calc R U . . .
C56 C 0.5672(8) 0.5591(8) 0.6507(4) 0.087(4) Uani 1 1 d . . . . .
H56A H 0.593832 0.617786 0.645712 0.130 Uiso 1 1 calc R U . . .
H56B H 0.581310 0.515975 0.632043 0.130 Uiso 1 1 calc R U . . .
H56C H 0.595471 0.538186 0.675007 0.130 Uiso 1 1 calc R U . . .
C57 C 0.1556(8) 0.5555(8) 0.5581(3) 0.075(3) Uani 1 1 d . . . . .
H57A H 0.130707 0.535284 0.580890 0.090 Uiso 1 1 calc R U . . .
C58 C 0.1466(9) 0.4765(10) 0.5306(4) 0.105(5) Uani 1 1 d . . . . .
H58A H 0.159656 0.497902 0.506592 0.157 Uiso 1 1 calc R U . . .
H58B H 0.082179 0.451980 0.528369 0.157 Uiso 1 1 calc R U . . .
H58C H 0.192422 0.429653 0.539470 0.157 Uiso 1 1 calc R U . . .
C59 C 0.0949(12) 0.6359(11) 0.5420(4) 0.121(6) Uani 1 1 d . . . . .
H59A H 0.098250 0.640501 0.515659 0.181 Uiso 1 1 calc R U . . .
H59B H 0.119090 0.691265 0.554253 0.181 Uiso 1 1 calc R U . . .
H59C H 0.028753 0.626721 0.545998 0.181 Uiso 1 1 calc R U . . .
C63 C 0.4323(4) 0.3051(5) 0.52079(15) 0.058(2) Uani 1 1 d G . . . .
C62 C 0.4309(4) 0.2098(5) 0.52065(15) 0.061(3) Uani 1 1 d G . . . .
C61 C 0.5219(5) 0.1791(3) 0.53638(16) 0.054(2) Uani 1 1 d G . . . .
C65 C 0.5796(3) 0.2554(4) 0.54624(14) 0.0514(18) Uani 1 1 d G . . . .
C64 C 0.5243(4) 0.3333(3) 0.53660(17) 0.057(2) Uani 1 1 d G . . . .
C66 C 0.5516(10) 0.0834(7) 0.5390(3) 0.082(4) Uani 1 1 d . . . . .
H66A H 0.602512 0.075877 0.559521 0.123 Uiso 1 1 calc R U . . .
H66B H 0.574541 0.065343 0.516104 0.123 Uiso 1 1 calc R U . . .
H66C H 0.497280 0.045952 0.542991 0.123 Uiso 1 1 calc R U . . .
C67 C 0.3481(9) 0.1501(9) 0.5054(3) 0.084(4) Uani 1 1 d . . . . .
H67A H 0.362815 0.087614 0.512234 0.126 Uiso 1 1 calc R U . . .
H67B H 0.337387 0.155326 0.478563 0.126 Uiso 1 1 calc R U . . .
H67C H 0.290873 0.168947 0.515449 0.126 Uiso 1 1 calc R U . . .
C68 C 0.3527(8) 0.3663(9) 0.5041(3) 0.086(4) Uani 1 1 d . . . . .
H68A H 0.291535 0.336606 0.504899 0.129 Uiso 1 1 calc R U . . .
H68B H 0.360416 0.379219 0.478504 0.129 Uiso 1 1 calc R U . . .
H68C H 0.354796 0.422500 0.517977 0.129 Uiso 1 1 calc R U . . .
C69 C 0.5582(8) 0.4300(6) 0.5410(3) 0.067(3) Uani 1 1 d . . . . .
H69A H 0.504135 0.469159 0.543683 0.100 Uiso 1 1 calc R U . . .
H69B H 0.586724 0.448074 0.519361 0.100 Uiso 1 1 calc R U . . .
H69C H 0.605500 0.435023 0.562929 0.100 Uiso 1 1 calc R U . . .
C70 C 0.6846(6) 0.2558(7) 0.5602(2) 0.063(2) Uani 1 1 d . . . . .
H70A H 0.702099 0.199059 0.572829 0.095 Uiso 1 1 calc R U . . .
H70B H 0.699088 0.305815 0.577344 0.095 Uiso 1 1 calc R U . . .
H70C H 0.720735 0.262721 0.539488 0.095 Uiso 1 1 calc R U . . .
C71 C 0.3552(5) 0.1946(5) 0.59911(19) 0.0376(15) Uani 1 1 d . . . . .
H71A H 0.320618 0.155197 0.581903 0.045 Uiso 1 1 calc R U . . .
O71 O 0.3262(4) 0.1947(3) 0.63113(13) 0.0396(11) Uani 1 1 d . . . . .
C72 C 0.4991(5) 0.3273(4) 0.62284(19) 0.0354(15) Uani 1 1 d . . . . .
H72A H 0.552392 0.364099 0.620274 0.042 Uiso 1 1 calc R U . . .
O72 O 0.4699(4) 0.3329(3) 0.65517(13) 0.0381(11) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C72 1.909(7) . ?
Ir1 C71 1.915(7) . ?
Ir1 C63 2.268(5) . ?
Ir1 C64 2.280(6) . ?
Ir1 C62 2.286(5) . ?
Ir1 C65 2.306(5) . ?
Ir1 C61 2.310(6) . ?
Ir1 Ca1 3.1944(14) . ?
Ir1 Ca2 3.2237(15) . ?
Ca1 O71 2.320(5) . ?
Ca1 O72 2.359(5) . ?
Ca1 N1 2.365(6) . ?
Ca1 N3 2.372(6) . ?
Ca2 O72 2.315(5) . ?
Ca2 O71 2.358(5) . ?
Ca2 N33 2.361(6) . ?
Ca2 N31 2.365(7) . ?
N1 C1 1.323(9) . ?
N1 C6 1.428(9) . ?
C1 C2 1.432(11) . ?
C1 C4 1.517(10) . ?
C2 C3 1.403(11) . ?
C3 N3 1.311(9) . ?
C3 C5 1.521(10) . ?
N3 C18 1.426(10) . ?
C6 C7 1.413(11) . ?
C6 C11 1.432(11) . ?
C7 C8 1.394(11) . ?
C7 C12 1.525(11) . ?
C8 C9 1.381(13) . ?
C9 C10 1.337(13) . ?
C10 C11 1.407(11) . ?
C11 C15 1.496(12) . ?
C12 C14 1.533(13) . ?
C12 C13 1.543(12) . ?
C15 C17 1.510(12) . ?
C15 C16 1.528(13) . ?
C18 C23 1.390(12) . ?
C18 C19 1.421(12) . ?
C19 C20 1.400(13) . ?
C19 C24 1.522(13) . ?
C20 C21 1.414(16) . ?
C21 C22 1.341(15) . ?
C22 C23 1.414(12) . ?
C23 C27 1.523(13) . ?
C24 C25 1.504(13) . ?
C24 C26 1.512(14) . ?
C27 C28 1.545(16) . ?
C27 C29 1.546(14) . ?
N31 C31 1.329(10) . ?
N31 C36 1.434(10) . ?
C31 C32 1.391(12) . ?
C31 C34 1.539(12) . ?
C32 C33 1.409(12) . ?
C33 N33 1.330(10) . ?
C33 C35 1.532(11) . ?
N33 C48 1.429(10) . ?
C36 C41 1.403(12) . ?
C36 C37 1.414(11) . ?
C37 C38 1.390(12) . ?
C37 C42 1.510(12) . ?
C38 C39 1.368(15) . ?
C39 C40 1.388(14) . ?
C40 C41 1.391(13) . ?
C41 C45 1.552(12) . ?
C42 C43 1.519(13) . ?
C42 C44 1.540(13) . ?
C45 C46 1.512(13) . ?
C45 C47 1.527(13) . ?
C48 C53 1.396(12) . ?
C48 C49 1.421(13) . ?
C49 C50 1.386(12) . ?
C49 C54 1.525(14) . ?
C50 C51 1.409(17) . ?
C51 C52 1.352(18) . ?
C52 C53 1.370(14) . ?
C53 C57 1.544(15) . ?
C54 C55 1.492(14) . ?
C54 C56 1.493(15) . ?
C57 C58 1.545(16) . ?
C57 C59 1.546(16) . ?
C63 C64 1.4200 . ?
C63 C62 1.4200 . ?
C63 C68 1.517(11) . ?
C62 C61 1.4200 . ?
C62 C67 1.521(12) . ?
C61 C65 1.4200 . ?
C61 C66 1.486(11) . ?
C65 C64 1.4200 . ?
C65 C70 1.512(10) . ?
C64 C69 1.521(11) . ?
C71 O71 1.299(8) . ?
C72 O72 1.314(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C72 Ir1 C71 98.4(3) . . ?
C72 Ir1 C63 128.1(3) . . ?
C71 Ir1 C63 119.4(3) . . ?
C72 Ir1 C64 101.0(3) . . ?
C71 Ir1 C64 155.8(3) . . ?
C63 Ir1 C64 36.39(8) . . ?
C72 Ir1 C62 161.4(2) . . ?
C71 Ir1 C62 99.8(2) . . ?
C63 Ir1 C62 36.34(7) . . ?
C64 Ir1 C62 60.42(8) . . ?
C72 Ir1 C65 105.2(3) . . ?
C71 Ir1 C65 147.8(3) . . ?
C63 Ir1 C65 60.31(9) . . ?
C64 Ir1 C65 36.07(7) . . ?
C62 Ir1 C65 60.05(8) . . ?
C72 Ir1 C61 136.4(3) . . ?
C71 Ir1 C61 113.1(3) . . ?
C63 Ir1 C61 60.25(8) . . ?
C64 Ir1 C61 60.08(8) . . ?
C62 Ir1 C61 35.99(8) . . ?
C65 Ir1 C61 35.84(7) . . ?
C72 Ir1 Ca1 57.28(19) . . ?
C71 Ir1 Ca1 57.3(2) . . ?
C63 Ir1 Ca1 174.56(19) . . ?
C64 Ir1 Ca1 146.78(16) . . ?
C62 Ir1 Ca1 138.34(18) . . ?
C65 Ir1 Ca1 119.68(12) . . ?
C61 Ir1 Ca1 116.17(13) . . ?
C72 Ir1 Ca2 57.5(2) . . ?
C71 Ir1 Ca2 57.3(2) . . ?
C63 Ir1 Ca2 113.74(13) . . ?
C64 Ir1 Ca2 123.75(15) . . ?
C62 Ir1 Ca2 131.52(15) . . ?
C65 Ir1 Ca2 154.88(17) . . ?
C61 Ir1 Ca2 166.06(16) . . ?
Ca1 Ir1 Ca2 68.73(4) . . ?
O71 Ca1 O72 78.18(18) . . ?
O71 Ca1 N1 139.0(2) . . ?
O72 Ca1 N1 89.81(19) . . ?
O71 Ca1 N3 109.8(2) . . ?
O72 Ca1 N3 171.5(2) . . ?
N1 Ca1 N3 82.2(2) . . ?
O72 Ca2 O71 78.30(18) . . ?
O72 Ca2 N33 112.6(2) . . ?
O71 Ca2 N33 168.5(2) . . ?
O72 Ca2 N31 133.9(2) . . ?
O71 Ca2 N31 88.3(2) . . ?
N33 Ca2 N31 81.5(2) . . ?
C1 N1 C6 118.7(6) . . ?
C1 N1 Ca1 125.2(5) . . ?
C6 N1 Ca1 116.0(4) . . ?
N1 C1 C2 125.0(6) . . ?
N1 C1 C4 120.7(7) . . ?
C2 C1 C4 114.3(6) . . ?
C3 C2 C1 130.9(6) . . ?
N3 C3 C2 126.3(7) . . ?
N3 C3 C5 120.7(7) . . ?
C2 C3 C5 112.9(6) . . ?
C3 N3 C18 119.9(6) . . ?
C3 N3 Ca1 124.4(5) . . ?
C18 N3 Ca1 115.7(4) . . ?
C7 C6 N1 118.6(7) . . ?
C7 C6 C11 120.5(7) . . ?
N1 C6 C11 120.8(7) . . ?
C8 C7 C6 118.7(7) . . ?
C8 C7 C12 119.3(7) . . ?
C6 C7 C12 122.0(7) . . ?
C9 C8 C7 120.5(8) . . ?
C10 C9 C8 120.8(8) . . ?
C9 C10 C11 123.0(9) . . ?
C10 C11 C6 116.3(8) . . ?
C10 C11 C15 121.1(8) . . ?
C6 C11 C15 122.6(7) . . ?
C7 C12 C14 113.2(7) . . ?
C7 C12 C13 110.3(7) . . ?
C14 C12 C13 110.6(8) . . ?
C11 C15 C17 112.4(8) . . ?
C11 C15 C16 111.3(8) . . ?
C17 C15 C16 109.7(7) . . ?
C23 C18 C19 120.7(8) . . ?
C23 C18 N3 119.8(7) . . ?
C19 C18 N3 119.5(8) . . ?
C20 C19 C18 117.6(9) . . ?
C20 C19 C24 120.3(9) . . ?
C18 C19 C24 122.0(8) . . ?
C19 C20 C21 121.0(10) . . ?
C22 C21 C20 120.2(9) . . ?
C21 C22 C23 120.9(10) . . ?
C18 C23 C22 119.4(9) . . ?
C18 C23 C27 123.2(8) . . ?
C22 C23 C27 117.3(9) . . ?
C25 C24 C26 110.8(9) . . ?
C25 C24 C19 112.2(8) . . ?
C26 C24 C19 113.0(9) . . ?
C23 C27 C28 110.5(8) . . ?
C23 C27 C29 112.3(9) . . ?
C28 C27 C29 111.8(9) . . ?
C31 N31 C36 116.9(7) . . ?
C31 N31 Ca2 125.0(5) . . ?
C36 N31 Ca2 118.0(5) . . ?
N31 C31 C32 126.8(8) . . ?
N31 C31 C34 119.0(8) . . ?
C32 C31 C34 114.1(8) . . ?
C31 C32 C33 130.9(7) . . ?
N33 C33 C32 124.3(7) . . ?
N33 C33 C35 120.8(8) . . ?
C32 C33 C35 114.8(7) . . ?
C33 N33 C48 118.5(7) . . ?
C33 N33 Ca2 126.5(5) . . ?
C48 N33 Ca2 115.0(5) . . ?
C41 C36 C37 118.7(8) . . ?
C41 C36 N31 121.8(7) . . ?
C37 C36 N31 119.5(7) . . ?
C38 C37 C36 120.0(8) . . ?
C38 C37 C42 118.8(8) . . ?
C36 C37 C42 121.1(8) . . ?
C39 C38 C37 120.6(9) . . ?
C38 C39 C40 120.1(9) . . ?
C39 C40 C41 120.7(9) . . ?
C40 C41 C36 119.6(9) . . ?
C40 C41 C45 120.3(8) . . ?
C36 C41 C45 120.1(8) . . ?
C37 C42 C43 112.7(9) . . ?
C37 C42 C44 113.6(9) . . ?
C43 C42 C44 108.1(8) . . ?
C46 C45 C47 110.1(8) . . ?
C46 C45 C41 111.6(8) . . ?
C47 C45 C41 110.9(8) . . ?
C53 C48 C49 119.7(8) . . ?
C53 C48 N33 121.2(9) . . ?
C49 C48 N33 118.9(7) . . ?
C53 C48 Ca2 119.3(6) . . ?
C49 C48 Ca2 102.3(5) . . ?
N33 C48 Ca2 41.4(3) . . ?
C50 C49 C48 117.3(9) . . ?
C50 C49 C54 120.0(10) . . ?
C48 C49 C54 122.7(8) . . ?
C49 C50 C51 121.9(12) . . ?
C52 C51 C50 119.0(10) . . ?
C51 C52 C53 121.4(10) . . ?
C52 C53 C48 120.6(11) . . ?
C52 C53 C57 118.8(9) . . ?
C48 C53 C57 120.6(8) . . ?
C55 C54 C56 109.2(9) . . ?
C55 C54 C49 111.7(9) . . ?
C56 C54 C49 115.8(9) . . ?
C53 C57 C58 109.7(9) . . ?
C53 C57 C59 112.3(11) . . ?
C58 C57 C59 110.3(10) . . ?
C64 C63 C62 108.0 . . ?
C64 C63 C68 125.7(7) . . ?
C62 C63 C68 126.1(7) . . ?
C64 C63 Ir1 72.3(2) . . ?
C62 C63 Ir1 72.5(2) . . ?
C68 C63 Ir1 124.8(5) . . ?
C61 C62 C63 108.0 . . ?
C61 C62 C67 125.4(7) . . ?
C63 C62 C67 126.6(7) . . ?
C61 C62 Ir1 72.9(2) . . ?
C63 C62 Ir1 71.1(2) . . ?
C67 C62 Ir1 123.1(5) . . ?
C65 C61 C62 108.0 . . ?
C65 C61 C66 127.0(7) . . ?
C62 C61 C66 124.8(7) . . ?
C65 C61 Ir1 71.9(2) . . ?
C62 C61 Ir1 71.10(19) . . ?
C66 C61 Ir1 126.2(6) . . ?
C61 C65 C64 108.0 . . ?
C61 C65 C70 126.8(6) . . ?
C64 C65 C70 124.8(6) . . ?
C61 C65 Ir1 72.2(2) . . ?
C64 C65 Ir1 71.0(2) . . ?
C70 C65 Ir1 128.0(4) . . ?
C63 C64 C65 108.0 . . ?
C63 C64 C69 125.8(6) . . ?
C65 C64 C69 126.2(6) . . ?
C63 C64 Ir1 71.33(19) . . ?
C65 C64 Ir1 73.0(2) . . ?
C69 C64 Ir1 123.1(5) . . ?
O71 C71 Ir1 132.1(5) . . ?
O71 C71 Ca1 59.3(4) . . ?
Ir1 C71 Ca1 85.9(3) . . ?
O71 C71 Ca2 60.1(4) . . ?
Ir1 C71 Ca2 86.4(2) . . ?
Ca1 C71 Ca2 84.0(2) . . ?
C71 O71 Ca1 91.9(4) . . ?
C71 O71 Ca2 91.3(4) . . ?
Ca1 O71 Ca2 101.5(2) . . ?
O72 C72 Ir1 131.9(5) . . ?
O72 C72 Ca1 61.1(3) . . ?
Ir1 C72 Ca1 86.1(2) . . ?
O72 C72 Ca2 58.1(3) . . ?
Ir1 C72 Ca2 86.3(2) . . ?
Ca1 C72 Ca2 83.9(2) . . ?
C72 O72 Ca2 93.1(4) . . ?
C72 O72 Ca1 89.7(4) . . ?
Ca2 O72 Ca1 101.6(2) . . ?

_refine_diff_density_max         2.585
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.123




# start Validation Reply Form
_vrf_RINTA01_3-Rh                
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: ...
The high angle scattering was very weak, with almost no data observed beyond
1.10 A resolution. See the supporting information for more details.
;
_vrf_PLAT020_3-Rh                
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.317 Report
RESPONSE: ...
See _vrf_RINTA01_3-Rh above
;
_vrf_PLAT026_3-Rh                
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        28% Check 
RESPONSE: ...
See _vrf_RINTA01_3-Rh above
;
_vrf_PLAT971_3-Ir                
;
PROBLEM: Check Calcd Resid. Dens.  1.15Ang From Ir1             2.58 eA-3  
RESPONSE: ...
The crystal studied was found to be severely twinned, with the best results
coming from modelling the crystal as a two component twin and then only
using data from the major component. Though the two residual electron
density peaks that are significantly larger than the rest are both ca. 1 A
away from the iridium centre in a pattern often seen around highly
absorbing atoms, their somewhat larger than typical magnitude is likely a
result of a combination of both absorption and the imperfectly resolved
twinning. See the supporting information for more details.
;
# end Validation Reply Form
#===END




