# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_B22302_a
_database_code_depnum_ccdc_archive 'CCDC 2283060'
loop_
_audit_author_name
_audit_author_address
'Jeffery A. Bertke'
;Georgetown University
United States of America
;
_audit_update_record             
;
2023-10-29 deposited with the CCDC.	2024-02-12 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         
;
C73.20 H112.40 Br0.10 Mg0.95 N7.80 Ni2 O3.80, 2(C5 H12)
;
_chemical_formula_sum            'C83.20 H136.40 Br0.10 Mg0.95 N7.80 Ni2 O3.80'
_chemical_formula_weight         1455.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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                   14.0458(7)
_cell_length_b                   15.2331(8)
_cell_length_c                   19.6481(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.204(2)
_cell_angle_gamma                90
_cell_volume                     4203.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9962
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      25.38
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_F_000             1583
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.601
_exptl_crystal_size_mid          0.468
_exptl_crystal_size_min          0.308
_exptl_absorpt_coefficient_mu    0.553
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66672
_exptl_absorpt_correction_T_max  0.81484
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            65731
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.800
_diffrn_reflns_theta_max         25.399
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7713
_reflns_number_gt                6872
_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.
 
 _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       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice was 
confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The final map had no significant features.  A final 
analysis of variance between observed and calculated structure factors showed 
little dependence on amplitude and resolution. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0447P)²+7.6274P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_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         7713
_refine_ls_number_parameters     609
_refine_ls_number_restraints     532
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.1149
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.056
_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
Ni1 Ni 0.73083(2) 0.76275(2) 0.47848(2) 0.01505(10) Uani 1 1 d . . . . .
N1 N 0.77664(13) 0.69613(12) 0.40346(9) 0.0120(4) Uani 1 1 d . . . . .
N2 N 0.81297(13) 0.70625(12) 0.54375(9) 0.0118(4) Uani 1 1 d . . . . .
N3 N 0.6495(3) 0.8434(2) 0.48399(18) 0.0226(8) Uani 0.515(3) 1 d D U P A 1
N4 N 0.5942(4) 0.8959(4) 0.4858(4) 0.0333(13) Uani 0.515(3) 1 d D U P A 1
Mg1 Mg 0.500000 1.000000 0.500000 0.0172(3) Uani 0.515(3) 2 d DS U P A 1
O1 O 0.4404(11) 0.9792(6) 0.4027(4) 0.0288(17) Uani 0.515(3) 1 d D U P A 1
C30 C 0.4403(6) 0.8976(5) 0.3654(3) 0.0377(18) Uani 0.515(3) 1 d D U P A 1
H30A H 0.505008 0.871692 0.366214 0.045 Uiso 0.515(3) 1 calc R U P A 1
H30B H 0.396185 0.855240 0.386332 0.045 Uiso 0.515(3) 1 calc R U P A 1
C31 C 0.4106(7) 0.9159(5) 0.2973(4) 0.0475(16) Uani 0.515(3) 1 d D U P A 1
H31A H 0.341885 0.903249 0.290740 0.057 Uiso 0.515(3) 1 calc R U P A 1
H31B H 0.446809 0.879723 0.264936 0.057 Uiso 0.515(3) 1 calc R U P A 1
C32 C 0.4305(13) 1.0134(5) 0.2862(4) 0.0420(19) Uani 0.515(3) 1 d D U P A 1
H32A H 0.497321 1.023590 0.273200 0.050 Uiso 0.515(3) 1 calc R U P A 1
H32B H 0.387207 1.038630 0.250870 0.050 Uiso 0.515(3) 1 calc R U P A 1
C33 C 0.4109(6) 1.0506(5) 0.3555(4) 0.0323(18) Uani 0.515(3) 1 d D U P A 1
H33A H 0.448644 1.104442 0.364073 0.039 Uiso 0.515(3) 1 calc R U P A 1
H33B H 0.342440 1.064402 0.360035 0.039 Uiso 0.515(3) 1 calc R U P A 1
O2 O 0.4021(8) 0.9139(5) 0.5459(8) 0.0223(17) Uani 0.515(3) 1 d D U P A 1
C34 C 0.3322(6) 0.9419(5) 0.5955(5) 0.0268(19) Uani 0.515(3) 1 d D U P A 1
H34A H 0.274047 0.964247 0.571914 0.032 Uiso 0.515(3) 1 calc R U P A 1
H34B H 0.358820 0.989234 0.624665 0.032 Uiso 0.515(3) 1 calc R U P A 1
C35 C 0.3092(6) 0.8634(6) 0.6373(4) 0.0360(19) Uani 0.515(3) 1 d D U P A 1
H35A H 0.318432 0.876519 0.686367 0.043 Uiso 0.515(3) 1 calc R U P A 1
H35B H 0.242273 0.845248 0.629108 0.043 Uiso 0.515(3) 1 calc R U P A 1
C36 C 0.3715(5) 0.7967(5) 0.6174(3) 0.0319(14) Uani 0.515(3) 1 d D U P A 1
H36A H 0.336091 0.740850 0.611993 0.038 Uiso 0.515(3) 1 calc R U P A 1
H36B H 0.421715 0.788205 0.652921 0.038 Uiso 0.515(3) 1 calc R U P A 1
C37 C 0.4144(6) 0.8202(5) 0.5539(4) 0.037(2) Uani 0.515(3) 1 d D U P A 1
H37A H 0.382921 0.788492 0.515581 0.045 Uiso 0.515(3) 1 calc R U P A 1
H37B H 0.482940 0.804910 0.554839 0.045 Uiso 0.515(3) 1 calc R U P A 1
N3B N 0.6495(3) 0.8434(2) 0.48399(18) 0.0226(8) Uani 0.435(3) 1 d D U P A 2
N4B N 0.5942(4) 0.8959(4) 0.4858(4) 0.0333(13) Uani 0.435(3) 1 d D U P A 2
Mg1B Mg 0.500000 1.000000 0.500000 0.0172(3) Uani 0.435(3) 2 d DS U P A 2
O1B O 0.4448(12) 0.9772(8) 0.4008(4) 0.0276(19) Uani 0.435(3) 1 d D U P A 2
C30B C 0.4664(8) 0.9066(6) 0.3544(4) 0.040(2) Uani 0.435(3) 1 d D U P A 2
H30C H 0.532652 0.886282 0.362566 0.048 Uiso 0.435(3) 1 calc R U P A 2
H30D H 0.423089 0.856452 0.362074 0.048 Uiso 0.435(3) 1 calc R U P A 2
C31B C 0.4551(7) 0.9374(6) 0.2853(3) 0.0360(16) Uani 0.435(3) 1 d D U P A 2
H31C H 0.403566 0.904814 0.261269 0.043 Uiso 0.435(3) 1 calc R U P A 2
H31D H 0.514924 0.929460 0.260244 0.043 Uiso 0.435(3) 1 calc R U P A 2
C32B C 0.4299(15) 1.0353(6) 0.2906(5) 0.0382(19) Uani 0.435(3) 1 d D U P A 2
H32C H 0.487339 1.072696 0.287702 0.046 Uiso 0.435(3) 1 calc R U P A 2
H32D H 0.383338 1.052951 0.254636 0.046 Uiso 0.435(3) 1 calc R U P A 2
C33B C 0.3873(8) 1.0402(7) 0.3600(4) 0.038(2) Uani 0.435(3) 1 d D U P A 2
H33C H 0.392677 1.100271 0.378985 0.046 Uiso 0.435(3) 1 calc R U P A 2
H33D H 0.319350 1.022845 0.358342 0.046 Uiso 0.435(3) 1 calc R U P A 2
O2B O 0.4009(9) 0.9127(5) 0.5432(9) 0.0219(19) Uani 0.435(3) 1 d D U P A 2
C34B C 0.3178(7) 0.9424(6) 0.5801(6) 0.031(2) Uani 0.435(3) 1 d D U P A 2
H34C H 0.266685 0.961444 0.547973 0.037 Uiso 0.435(3) 1 calc R U P A 2
H34D H 0.334827 0.992128 0.610390 0.037 Uiso 0.435(3) 1 calc R U P A 2
C35B C 0.2862(6) 0.8654(6) 0.6207(5) 0.033(2) Uani 0.435(3) 1 d D U P A 2
H35C H 0.301187 0.874869 0.669596 0.040 Uiso 0.435(3) 1 calc R U P A 2
H35D H 0.216540 0.857162 0.615042 0.040 Uiso 0.435(3) 1 calc R U P A 2
C36B C 0.3344(7) 0.7916(5) 0.5970(5) 0.0409(18) Uani 0.435(3) 1 d D U P A 2
H36C H 0.288142 0.746244 0.581893 0.049 Uiso 0.435(3) 1 calc R U P A 2
H36D H 0.374973 0.766550 0.633961 0.049 Uiso 0.435(3) 1 calc R U P A 2
C37B C 0.3936(6) 0.8182(5) 0.5398(4) 0.0210(18) Uani 0.435(3) 1 d D U P A 2
H37C H 0.457513 0.791015 0.543806 0.025 Uiso 0.435(3) 1 calc R U P A 2
H37D H 0.363639 0.799867 0.495988 0.025 Uiso 0.435(3) 1 calc R U P A 2
Br1 Br 0.6199(10) 0.8769(12) 0.4886(10) 0.041(4) Uani 0.05 1 d . U P A 3
C1 C 0.8700(2) 0.58681(17) 0.34093(12) 0.0222(6) Uani 1 1 d . . . . .
H1A H 0.913781 0.538608 0.352094 0.033 Uiso 1 1 calc R U . . .
H1B H 0.901417 0.628663 0.310905 0.033 Uiso 1 1 calc R U . . .
H1C H 0.812934 0.563319 0.317838 0.033 Uiso 1 1 calc R U . . .
C2 C 0.84183(17) 0.63290(15) 0.40568(12) 0.0144(5) Uani 1 1 d . . . . .
C3 C 0.88788(17) 0.60764(15) 0.46642(12) 0.0159(5) Uani 1 1 d . . . . .
H3 H 0.932636 0.561157 0.463153 0.019 Uiso 1 1 calc R U . . .
C4 C 0.87561(16) 0.64302(15) 0.53166(12) 0.0139(5) Uani 1 1 d . . . . .
C5 C 0.93680(18) 0.60601(17) 0.58915(13) 0.0201(5) Uani 1 1 d . . . . .
H5A H 0.987426 0.569671 0.570283 0.030 Uiso 1 1 calc R U . . .
H5B H 0.897381 0.570078 0.618853 0.030 Uiso 1 1 calc R U . . .
H5C H 0.965217 0.654308 0.615516 0.030 Uiso 1 1 calc R U . . .
C6 C 0.73904(16) 0.72721(15) 0.33986(11) 0.0132(5) Uani 1 1 d . . . . .
C7 C 0.78979(17) 0.79142(15) 0.30400(12) 0.0158(5) Uani 1 1 d . . . . .
C8 C 0.74678(19) 0.82888(16) 0.24643(13) 0.0201(5) Uani 1 1 d . . . . .
H8 H 0.779735 0.873017 0.222175 0.024 Uiso 1 1 calc R U . . .
C9 C 0.65721(19) 0.80318(18) 0.22388(13) 0.0234(6) Uani 1 1 d . . . . .
H9 H 0.629014 0.829580 0.184564 0.028 Uiso 1 1 calc R U . . .
C10 C 0.60866(18) 0.73872(17) 0.25886(13) 0.0213(5) Uani 1 1 d . . . . .
H10 H 0.547294 0.720924 0.242989 0.026 Uiso 1 1 calc R U . . .
C11 C 0.64841(17) 0.69957(16) 0.31697(12) 0.0169(5) Uani 1 1 d . . . . .
C12 C 0.88578(17) 0.82384(17) 0.33094(13) 0.0198(5) Uani 1 1 d . . . . .
H12 H 0.909194 0.780303 0.365510 0.024 Uiso 1 1 calc R U . . .
C13 C 0.96084(19) 0.8295(2) 0.27562(15) 0.0295(6) Uani 1 1 d . . . . .
H13A H 1.021215 0.850044 0.295793 0.044 Uiso 1 1 calc R U . . .
H13B H 0.939357 0.870654 0.240195 0.044 Uiso 1 1 calc R U . . .
H13C H 0.969955 0.771281 0.255488 0.044 Uiso 1 1 calc R U . . .
C14 C 0.8745(2) 0.91158(18) 0.36740(15) 0.0291(6) Uani 1 1 d . . . . .
H14A H 0.936588 0.930794 0.385647 0.044 Uiso 1 1 calc R U . . .
H14B H 0.830064 0.904780 0.404806 0.044 Uiso 1 1 calc R U . . .
H14C H 0.849772 0.955500 0.335178 0.044 Uiso 1 1 calc R U . . .
C15 C 0.59526(18) 0.62825(16) 0.35476(13) 0.0200(5) Uani 1 1 d . . . . .
H15 H 0.636739 0.609107 0.393999 0.024 Uiso 1 1 calc R U . . .
C16 C 0.5780(2) 0.54830(17) 0.30936(15) 0.0284(6) Uani 1 1 d . . . . .
H16A H 0.551066 0.500634 0.336352 0.043 Uiso 1 1 calc R U . . .
H16B H 0.638506 0.529094 0.290319 0.043 Uiso 1 1 calc R U . . .
H16C H 0.533457 0.563826 0.272248 0.043 Uiso 1 1 calc R U . . .
C17 C 0.5019(2) 0.66175(19) 0.38374(15) 0.0294(6) Uani 1 1 d . . . . .
H17A H 0.470623 0.614153 0.408306 0.044 Uiso 1 1 calc R U . . .
H17B H 0.459985 0.682034 0.346449 0.044 Uiso 1 1 calc R U . . .
H17C H 0.515169 0.710535 0.415030 0.044 Uiso 1 1 calc R U . . .
C18 C 0.80399(16) 0.73889(15) 0.61138(11) 0.0128(5) Uani 1 1 d . . . . .
C19 C 0.85028(17) 0.81741(16) 0.62971(12) 0.0161(5) Uani 1 1 d . . . . .
C20 C 0.83831(18) 0.84977(16) 0.69535(13) 0.0203(5) Uani 1 1 d . . . . .
H20 H 0.870072 0.902205 0.708853 0.024 Uiso 1 1 calc R U . . .
C21 C 0.78085(19) 0.80682(17) 0.74137(13) 0.0232(6) Uani 1 1 d . . . . .
H21 H 0.773730 0.829728 0.785941 0.028 Uiso 1 1 calc R U . . .
C22 C 0.73385(19) 0.73036(17) 0.72209(13) 0.0219(5) Uani 1 1 d . . . . .
H22 H 0.693844 0.701745 0.753547 0.026 Uiso 1 1 calc R U . . .
C23 C 0.74441(17) 0.69487(16) 0.65726(12) 0.0164(5) Uani 1 1 d . . . . .
C24 C 0.91067(19) 0.86711(17) 0.57890(12) 0.0207(5) Uani 1 1 d . . . . .
H24 H 0.902470 0.837344 0.533791 0.025 Uiso 1 1 calc R U . . .
C25 C 1.0162(2) 0.8643(2) 0.59804(16) 0.0329(7) Uani 1 1 d . . . . .
H25A H 1.052577 0.894725 0.563146 0.049 Uiso 1 1 calc R U . . .
H25B H 1.037251 0.803100 0.601228 0.049 Uiso 1 1 calc R U . . .
H25C H 1.026697 0.893352 0.642072 0.049 Uiso 1 1 calc R U . . .
C26 C 0.8771(2) 0.96149(19) 0.57026(17) 0.0334(7) Uani 1 1 d . . . . .
H26A H 0.915251 0.990714 0.535762 0.050 Uiso 1 1 calc R U . . .
H26B H 0.884431 0.992629 0.613699 0.050 Uiso 1 1 calc R U . . .
H26C H 0.809889 0.961929 0.555753 0.050 Uiso 1 1 calc R U . . .
C27 C 0.68988(18) 0.61365(16) 0.63429(13) 0.0199(5) Uani 1 1 d . . . . .
H27 H 0.727667 0.585000 0.597880 0.024 Uiso 1 1 calc R U . . .
C28 C 0.5939(2) 0.63971(19) 0.60231(14) 0.0281(6) Uani 1 1 d . . . . .
H28A H 0.561353 0.587204 0.584756 0.042 Uiso 1 1 calc R U . . .
H28B H 0.604060 0.680938 0.564874 0.042 Uiso 1 1 calc R U . . .
H28C H 0.554590 0.667685 0.636783 0.042 Uiso 1 1 calc R U . . .
C29 C 0.67703(19) 0.54588(17) 0.69066(14) 0.0244(6) Uani 1 1 d . . . . .
H29A H 0.650152 0.491893 0.671102 0.037 Uiso 1 1 calc R U . . .
H29B H 0.633765 0.569273 0.724687 0.037 Uiso 1 1 calc R U . . .
H29C H 0.738928 0.532998 0.712344 0.037 Uiso 1 1 calc R U . . .
C38 C 0.7005(12) 0.4315(11) 0.4641(6) 0.051(3) Uani 0.619(6) 1 d D U P B 1
H38A H 0.704828 0.439488 0.414760 0.076 Uiso 0.619(6) 1 calc R U P B 1
H38B H 0.701703 0.488948 0.486537 0.076 Uiso 0.619(6) 1 calc R U P B 1
H38C H 0.640980 0.401235 0.474400 0.076 Uiso 0.619(6) 1 calc R U P B 1
C39 C 0.7849(4) 0.3766(4) 0.4899(3) 0.0424(14) Uani 0.619(6) 1 d D U P B 1
H39A H 0.783237 0.319023 0.466633 0.051 Uiso 0.619(6) 1 calc R U P B 1
H39B H 0.844592 0.406471 0.477313 0.051 Uiso 0.619(6) 1 calc R U P B 1
C40 C 0.7868(4) 0.3616(4) 0.5651(3) 0.0393(12) Uani 0.619(6) 1 d D U P B 1
H40A H 0.724466 0.337182 0.578281 0.047 Uiso 0.619(6) 1 calc R U P B 1
H40B H 0.794608 0.418901 0.588289 0.047 Uiso 0.619(6) 1 calc R U P B 1
C41 C 0.8657(7) 0.2995(5) 0.5911(5) 0.044(2) Uani 0.619(6) 1 d D U P B 1
H41A H 0.925172 0.310874 0.566479 0.052 Uiso 0.619(6) 1 calc R U P B 1
H41B H 0.878273 0.309742 0.640253 0.052 Uiso 0.619(6) 1 calc R U P B 1
C42 C 0.8355(6) 0.2095(4) 0.5802(4) 0.0442(17) Uani 0.619(6) 1 d D U P B 1
H42A H 0.879663 0.169696 0.604093 0.066 Uiso 0.619(6) 1 calc R U P B 1
H42B H 0.835255 0.196361 0.531319 0.066 Uiso 0.619(6) 1 calc R U P B 1
H42C H 0.771258 0.201497 0.597635 0.066 Uiso 0.619(6) 1 calc R U P B 1
C38B C 0.6905(17) 0.4438(16) 0.4797(10) 0.046(4) Uani 0.381(6) 1 d D U P B 2
H38D H 0.694648 0.414581 0.435369 0.069 Uiso 0.381(6) 1 calc R U P B 2
H38E H 0.725876 0.499185 0.478657 0.069 Uiso 0.381(6) 1 calc R U P B 2
H38F H 0.623586 0.455679 0.489432 0.069 Uiso 0.381(6) 1 calc R U P B 2
C39B C 0.7331(6) 0.3844(6) 0.5350(4) 0.0389(19) Uani 0.381(6) 1 d D U P B 2
H39C H 0.729246 0.414982 0.579271 0.047 Uiso 0.381(6) 1 calc R U P B 2
H39D H 0.693865 0.330547 0.537685 0.047 Uiso 0.381(6) 1 calc R U P B 2
C40B C 0.8342(6) 0.3583(6) 0.5242(5) 0.0456(19) Uani 0.381(6) 1 d D U P B 2
H40C H 0.872378 0.412150 0.517774 0.055 Uiso 0.381(6) 1 calc R U P B 2
H40D H 0.837078 0.323699 0.481674 0.055 Uiso 0.381(6) 1 calc R U P B 2
C41B C 0.8801(13) 0.3046(9) 0.5819(9) 0.047(3) Uani 0.381(6) 1 d D U P B 2
H41C H 0.947135 0.323011 0.589263 0.057 Uiso 0.381(6) 1 calc R U P B 2
H41D H 0.845582 0.314364 0.624660 0.057 Uiso 0.381(6) 1 calc R U P B 2
C42B C 0.8763(11) 0.2130(9) 0.5635(9) 0.070(4) Uani 0.381(6) 1 d D U P B 2
H42D H 0.932324 0.182788 0.582612 0.105 Uiso 0.381(6) 1 calc R U P B 2
H42E H 0.875371 0.207426 0.513843 0.105 Uiso 0.381(6) 1 calc R U P B 2
H42F H 0.818443 0.186610 0.581677 0.105 Uiso 0.381(6) 1 calc R U P B 2


_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.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016).  Four 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2016) then corrected for absorption by integration using 
SAINT/SADABS v2014/2 (Bruker, 2016) to sort, merge, and scale the combined 
data.  No decay correction was applied.    
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 1.00 0.1780
1.00 1.00 0.00 0.2430
1.00 -1.00 0.00 0.1980
0.00 1.00 1.00 0.1930
2.00 -1.00 -2.00 0.2460
0.00 0.00 1.00 0.2260
0.00 0.00 -1.00 0.2340
2.00 -1.00 2.00 0.2890
-2.00 1.00 -2.00 0.2460
0.00 1.00 -1.00 0.2470
1.00 -2.00 0.00 0.1510
1.00 -2.00 -2.00 0.1520
0.00 1.00 0.00 0.1540
0.00 -1.00 0.00 0.0860
0.00 1.00 2.00 0.1910
0.00 -1.00 -2.00 0.1740
-2.00 0.00 1.00 0.1870

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
Ni1 N3B 1.682(4) . ?
Ni1 N3 1.682(4) . ?
Ni1 N2 1.9115(19) . ?
Ni1 N1 1.9122(18) . ?
Ni1 Br1 2.346(17) . ?
N1 C2 1.329(3) . ?
N1 C6 1.427(3) . ?
N2 C4 1.329(3) . ?
N2 C18 1.427(3) . ?
N3 N4 1.116(7) . ?
N4 Mg1 2.088(6) . ?
Mg1 O1 2.095(4) . ?
Mg1 O1 2.095(5) 3_676 ?
Mg1 O2 2.116(4) 3_676 ?
Mg1 O2 2.116(4) . ?
O1 C30 1.444(7) . ?
O1 C33 1.482(7) . ?
C30 C31 1.421(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.528(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.505(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O2 C37 1.446(6) . ?
O2 C34 1.461(6) . ?
C34 C35 1.491(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.401(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.443(7) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
N3B N4B 1.116(7) . ?
N4B Mg1B 2.088(6) . ?
Mg1B O1B 2.111(5) . ?
Mg1B O2B 2.115(5) . ?
O1B C30B 1.447(7) . ?
O1B C33B 1.480(7) . ?
C30B C31B 1.441(8) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C31B C32B 1.537(9) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C32B C33B 1.502(9) . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
C33B H33C 0.9900 . ?
C33B H33D 0.9900 . ?
O2B C37B 1.444(7) . ?
O2B C34B 1.459(7) . ?
C34B C35B 1.491(7) . ?
C34B H34C 0.9900 . ?
C34B H34D 0.9900 . ?
C35B C36B 1.398(8) . ?
C35B H35C 0.9900 . ?
C35B H35D 0.9900 . ?
C36B C37B 1.470(7) . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C1 C2 1.513(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.399(3) . ?
C3 C4 1.404(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.514(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.406(3) . ?
C6 C7 1.408(3) . ?
C7 C8 1.393(4) . ?
C7 C12 1.520(3) . ?
C8 C9 1.382(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(4) . ?
C10 H10 0.9500 . ?
C11 C15 1.521(3) . ?
C12 C14 1.526(4) . ?
C12 C13 1.532(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.526(4) . ?
C15 C17 1.528(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.405(3) . ?
C18 C23 1.412(3) . ?
C19 C20 1.394(3) . ?
C19 C24 1.525(3) . ?
C20 C21 1.388(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(3) . ?
C22 H22 0.9500 . ?
C23 C27 1.519(3) . ?
C24 C26 1.522(4) . ?
C24 C25 1.522(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.528(3) . ?
C27 C28 1.528(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C38 C39 1.528(9) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.495(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.536(8) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.450(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C38B C39B 1.527(11) . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
C39B C40B 1.494(8) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C40B C41B 1.529(10) . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
C41B C42B 1.441(9) . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?

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
N3B Ni1 N2 133.36(14) . . ?
N3 Ni1 N2 133.36(14) . . ?
N3B Ni1 N1 132.61(14) . . ?
N3 Ni1 N1 132.61(14) . . ?
N2 Ni1 N1 94.02(8) . . ?
N2 Ni1 Br1 132.0(5) . . ?
N1 Ni1 Br1 133.9(5) . . ?
C2 N1 C6 120.74(19) . . ?
C2 N1 Ni1 127.02(16) . . ?
C6 N1 Ni1 112.00(14) . . ?
C4 N2 C18 119.37(19) . . ?
C4 N2 Ni1 126.79(16) . . ?
C18 N2 Ni1 113.83(14) . . ?
N4 N3 Ni1 177.8(6) . . ?
N3 N4 Mg1 172.7(7) . . ?
N4 Mg1 N4 180.0 . 3_676 ?
N4 Mg1 O1 90.3(3) . . ?
N4 Mg1 O1 89.7(3) 3_676 . ?
N4 Mg1 O1 89.7(3) . 3_676 ?
N4 Mg1 O1 90.3(3) 3_676 3_676 ?
O1 Mg1 O1 180.0 . 3_676 ?
N4 Mg1 O2 89.7(3) . 3_676 ?
N4 Mg1 O2 90.3(3) 3_676 3_676 ?
O1 Mg1 O2 87.5(4) . 3_676 ?
O1 Mg1 O2 92.5(4) 3_676 3_676 ?
N4 Mg1 O2 90.3(3) . . ?
N4 Mg1 O2 89.7(3) 3_676 . ?
O1 Mg1 O2 92.5(4) . . ?
O1 Mg1 O2 87.5(4) 3_676 . ?
O2 Mg1 O2 180.0 3_676 . ?
C30 O1 C33 108.5(4) . . ?
C30 O1 Mg1 126.1(5) . . ?
C33 O1 Mg1 124.2(6) . . ?
C31 C30 O1 107.8(5) . . ?
C31 C30 H30A 110.1 . . ?
O1 C30 H30A 110.1 . . ?
C31 C30 H30B 110.1 . . ?
O1 C30 H30B 110.1 . . ?
H30A C30 H30B 108.5 . . ?
C30 C31 C32 105.9(6) . . ?
C30 C31 H31A 110.5 . . ?
C32 C31 H31A 110.5 . . ?
C30 C31 H31B 110.5 . . ?
C32 C31 H31B 110.5 . . ?
H31A C31 H31B 108.7 . . ?
C33 C32 C31 101.4(6) . . ?
C33 C32 H32A 111.5 . . ?
C31 C32 H32A 111.5 . . ?
C33 C32 H32B 111.5 . . ?
C31 C32 H32B 111.5 . . ?
H32A C32 H32B 109.3 . . ?
O1 C33 C32 103.7(5) . . ?
O1 C33 H33A 111.0 . . ?
C32 C33 H33A 111.0 . . ?
O1 C33 H33B 111.0 . . ?
C32 C33 H33B 111.0 . . ?
H33A C33 H33B 109.0 . . ?
C37 O2 C34 107.3(5) . . ?
C37 O2 Mg1 125.5(5) . . ?
C34 O2 Mg1 123.7(6) . . ?
O2 C34 C35 106.8(5) . . ?
O2 C34 H34A 110.4 . . ?
C35 C34 H34A 110.4 . . ?
O2 C34 H34B 110.4 . . ?
C35 C34 H34B 110.4 . . ?
H34A C34 H34B 108.6 . . ?
C36 C35 C34 106.5(5) . . ?
C36 C35 H35A 110.4 . . ?
C34 C35 H35A 110.4 . . ?
C36 C35 H35B 110.4 . . ?
C34 C35 H35B 110.4 . . ?
H35A C35 H35B 108.6 . . ?
C35 C36 C37 109.7(5) . . ?
C35 C36 H36A 109.7 . . ?
C37 C36 H36A 109.7 . . ?
C35 C36 H36B 109.7 . . ?
C37 C36 H36B 109.7 . . ?
H36A C36 H36B 108.2 . . ?
C36 C37 O2 106.7(5) . . ?
C36 C37 H37A 110.4 . . ?
O2 C37 H37A 110.4 . . ?
C36 C37 H37B 110.4 . . ?
O2 C37 H37B 110.4 . . ?
H37A C37 H37B 108.6 . . ?
N4B N3B Ni1 177.8(6) . . ?
N3B N4B Mg1B 172.7(7) . . ?
N4B Mg1B O1B 88.4(3) . . ?
N4B Mg1B O2B 90.0(3) . . ?
O1B Mg1B O2B 92.0(5) . . ?
C30B O1B C33B 105.1(5) . . ?
C30B O1B Mg1B 128.8(6) . . ?
C33B O1B Mg1B 125.4(6) . . ?
C31B C30B O1B 109.3(6) . . ?
C31B C30B H30C 109.8 . . ?
O1B C30B H30C 109.8 . . ?
C31B C30B H30D 109.8 . . ?
O1B C30B H30D 109.8 . . ?
H30C C30B H30D 108.3 . . ?
C30B C31B C32B 105.9(6) . . ?
C30B C31B H31C 110.6 . . ?
C32B C31B H31C 110.6 . . ?
C30B C31B H31D 110.6 . . ?
C32B C31B H31D 110.6 . . ?
H31C C31B H31D 108.7 . . ?
C33B C32B C31B 101.9(6) . . ?
C33B C32B H32C 111.4 . . ?
C31B C32B H32C 111.4 . . ?
C33B C32B H32D 111.4 . . ?
C31B C32B H32D 111.4 . . ?
H32C C32B H32D 109.3 . . ?
O1B C33B C32B 103.7(8) . . ?
O1B C33B H33C 111.0 . . ?
C32B C33B H33C 111.0 . . ?
O1B C33B H33D 111.0 . . ?
C32B C33B H33D 111.0 . . ?
H33C C33B H33D 109.0 . . ?
C37B O2B C34B 106.0(6) . . ?
C37B O2B Mg1B 130.9(5) . . ?
C34B O2B Mg1B 123.0(6) . . ?
O2B C34B C35B 105.9(6) . . ?
O2B C34B H34C 110.6 . . ?
C35B C34B H34C 110.6 . . ?
O2B C34B H34D 110.6 . . ?
C35B C34B H34D 110.6 . . ?
H34C C34B H34D 108.7 . . ?
C36B C35B C34B 107.6(6) . . ?
C36B C35B H35C 110.2 . . ?
C34B C35B H35C 110.2 . . ?
C36B C35B H35D 110.2 . . ?
C34B C35B H35D 110.2 . . ?
H35C C35B H35D 108.5 . . ?
C35B C36B C37B 108.6(6) . . ?
C35B C36B H36C 110.0 . . ?
C37B C36B H36C 110.0 . . ?
C35B C36B H36D 110.0 . . ?
C37B C36B H36D 110.0 . . ?
H36C C36B H36D 108.3 . . ?
O2B C37B C36B 106.3(5) . . ?
O2B C37B H37C 110.5 . . ?
C36B C37B H37C 110.5 . . ?
O2B C37B H37D 110.5 . . ?
C36B C37B H37D 110.5 . . ?
H37C C37B H37D 108.7 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 122.2(2) . . ?
N1 C2 C1 120.0(2) . . ?
C3 C2 C1 117.7(2) . . ?
C2 C3 C4 127.6(2) . . ?
C2 C3 H3 116.2 . . ?
C4 C3 H3 116.2 . . ?
N2 C4 C3 122.4(2) . . ?
N2 C4 C5 120.3(2) . . ?
C3 C4 C5 117.3(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 120.8(2) . . ?
C11 C6 N1 119.8(2) . . ?
C7 C6 N1 119.1(2) . . ?
C8 C7 C6 118.4(2) . . ?
C8 C7 C12 121.0(2) . . ?
C6 C7 C12 120.4(2) . . ?
C9 C8 C7 121.4(2) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 119.7(2) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C11 121.1(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C6 118.6(2) . . ?
C10 C11 C15 120.9(2) . . ?
C6 C11 C15 120.6(2) . . ?
C7 C12 C14 110.4(2) . . ?
C7 C12 C13 112.9(2) . . ?
C14 C12 C13 111.3(2) . . ?
C7 C12 H12 107.3 . . ?
C14 C12 H12 107.3 . . ?
C13 C12 H12 107.3 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C16 111.0(2) . . ?
C11 C15 C17 112.2(2) . . ?
C16 C15 C17 110.9(2) . . ?
C11 C15 H15 107.5 . . ?
C16 C15 H15 107.5 . . ?
C17 C15 H15 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 121.2(2) . . ?
C19 C18 N2 119.1(2) . . ?
C23 C18 N2 119.6(2) . . ?
C20 C19 C18 118.3(2) . . ?
C20 C19 C24 120.7(2) . . ?
C18 C19 C24 121.0(2) . . ?
C21 C20 C19 121.3(2) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C22 C21 C20 119.8(2) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 121.0(2) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C22 C23 C18 118.3(2) . . ?
C22 C23 C27 121.6(2) . . ?
C18 C23 C27 119.9(2) . . ?
C26 C24 C25 110.6(2) . . ?
C26 C24 C19 111.5(2) . . ?
C25 C24 C19 112.1(2) . . ?
C26 C24 H24 107.4 . . ?
C25 C24 H24 107.4 . . ?
C19 C24 H24 107.4 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C29 113.7(2) . . ?
C23 C27 C28 110.2(2) . . ?
C29 C27 C28 110.9(2) . . ?
C23 C27 H27 107.2 . . ?
C29 C27 H27 107.2 . . ?
C28 C27 H27 107.2 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C38 114.2(7) . . ?
C40 C39 H39A 108.7 . . ?
C38 C39 H39A 108.7 . . ?
C40 C39 H39B 108.7 . . ?
C38 C39 H39B 108.7 . . ?
H39A C39 H39B 107.6 . . ?
C39 C40 C41 114.9(6) . . ?
C39 C40 H40A 108.5 . . ?
C41 C40 H40A 108.5 . . ?
C39 C40 H40B 108.5 . . ?
C41 C40 H40B 108.5 . . ?
H40A C40 H40B 107.5 . . ?
C42 C41 C40 109.0(6) . . ?
C42 C41 H41A 109.9 . . ?
C40 C41 H41A 109.9 . . ?
C42 C41 H41B 109.9 . . ?
C40 C41 H41B 109.9 . . ?
H41A C41 H41B 108.3 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39B C38B H38D 109.5 . . ?
C39B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C39B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C40B C39B C38B 114.6(11) . . ?
C40B C39B H39C 108.6 . . ?
C38B C39B H39C 108.6 . . ?
C40B C39B H39D 108.6 . . ?
C38B C39B H39D 108.6 . . ?
H39C C39B H39D 107.6 . . ?
C39B C40B C41B 115.2(10) . . ?
C39B C40B H40C 108.5 . . ?
C41B C40B H40C 108.5 . . ?
C39B C40B H40D 108.5 . . ?
C41B C40B H40D 108.5 . . ?
H40C C40B H40D 107.5 . . ?
C42B C41B C40B 108.6(10) . . ?
C42B C41B H41C 110.0 . . ?
C40B C41B H41C 110.0 . . ?
C42B C41B H41D 110.0 . . ?
C40B C41B H41D 110.0 . . ?
H41C C41B H41D 108.4 . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

_refine_diff_density_max         0.656
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.063


_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive
####################################################################### 
# 
# 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_B22312_a
_database_code_depnum_ccdc_archive 'CCDC 2283061'
loop_
_audit_author_name
_audit_author_address
'Jeffery A. Bertke'
;Georgetown University
United States of America
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT230_B22312_a            
;
PROBLEM: Hirshfeld Test Diff for    N1       --N2       .       19.0 s.u.  
RESPONSE: It is not surprising that the components of the anisotropic 
displacement parameters along the bonds in this Ni-N-N-Ca moiety are not 
equal in magnitude.  We are confident that all atom assignments are correct.
;
_vrf_PLAT232_B22312_a            
;
PROBLEM: Hirshfeld Test Diff (M-X)  Ni1      --N1       .       23.5 s.u.  
RESPONSE: It is not surprising that the components of the anisotropic 
displacement parameters along the bonds in this Ni-N-N-Ca moiety are not 
equal in magnitude.  We are confident that all atom assignments are correct.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H114 Ca N8 Ni2 O4, 2(C5 H12)'
_chemical_formula_sum            'C84 H138 Ca N8 Ni2 O4'
_chemical_formula_weight         1481.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   14.0658(11)
_cell_length_b                   15.3664(13)
_cell_length_c                   19.8258(17)
_cell_angle_alpha                90
_cell_angle_beta                 91.419(3)
_cell_angle_gamma                90
_cell_volume                     4283.8(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9823
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      25.40
_exptl_crystal_description       Block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_F_000             1612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.716
_exptl_crystal_size_mid          0.690
_exptl_crystal_size_min          0.238
_exptl_absorpt_coefficient_mu    0.549
_shelx_estimated_absorpt_T_min   0.694
_shelx_estimated_absorpt_T_max   0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62299
_exptl_absorpt_correction_T_max  0.82365
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51802
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.755
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7866
_reflns_number_gt                6355
_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.
 
 _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       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2018-3 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice was 
confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The final map had no significant features.  A final 
analysis of variance between observed and calculated structure factors 
showed little dependence on amplitude and resolution. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0473P)²+8.8199P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_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         7866
_refine_ls_number_parameters     554
_refine_ls_number_restraints     294
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1329
_refine_ls_wR_factor_gt          0.1221
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.026
_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
Ni1 Ni 0.26058(2) 0.25330(2) 0.51914(2) 0.01962(11) Uani 1 1 d . . . . .
Ca1 Ca 0.500000 0.500000 0.500000 0.0274(2) Uani 1 2 d DS . P . .
N1 N 0.3425(2) 0.32969(19) 0.51648(12) 0.0318(6) Uani 1 1 d . . . . .
N2 N 0.4001(2) 0.38396(19) 0.51661(14) 0.0379(7) Uani 1 1 d . . . . .
N3 N 0.21428(17) 0.19071(15) 0.59456(11) 0.0201(5) Uani 1 1 d . . . . .
N4 N 0.17792(16) 0.19917(15) 0.45452(11) 0.0206(5) Uani 1 1 d . . . . .
C1 C 0.1186(2) 0.0864(2) 0.65741(15) 0.0312(7) Uani 1 1 d . . . . .
H1A H 0.074723 0.038583 0.646633 0.047 Uiso 1 1 calc R U . . .
H1B H 0.087128 0.128667 0.686388 0.047 Uiso 1 1 calc R U . . .
H1C H 0.175243 0.063361 0.681018 0.047 Uiso 1 1 calc R U . . .
C2 C 0.1475(2) 0.13050(18) 0.59301(14) 0.0220(6) Uani 1 1 d . . . . .
C3 C 0.1006(2) 0.10578(19) 0.53273(14) 0.0246(6) Uani 1 1 d . . . . .
H3 H 0.054894 0.060586 0.536399 0.029 Uiso 1 1 calc R U . . .
C4 C 0.1126(2) 0.13939(18) 0.46786(14) 0.0217(6) Uani 1 1 d . . . . .
C5 C 0.0496(2) 0.1044(2) 0.41139(15) 0.0300(7) Uani 1 1 d . . . . .
H5A H -0.006280 0.076341 0.430390 0.045 Uiso 1 1 calc R U . . .
H5B H 0.085092 0.061810 0.385209 0.045 Uiso 1 1 calc R U . . .
H5C H 0.029069 0.152414 0.381914 0.045 Uiso 1 1 calc R U . . .
C6 C 0.2537(2) 0.22310(18) 0.65717(13) 0.0201(6) Uani 1 1 d . . . . .
C7 C 0.3450(2) 0.19650(18) 0.67945(14) 0.0215(6) Uani 1 1 d . . . . .
C8 C 0.3869(2) 0.23736(19) 0.73552(15) 0.0256(6) Uani 1 1 d . . . . .
H8 H 0.448609 0.219917 0.750709 0.031 Uiso 1 1 calc R U . . .
C9 C 0.3404(2) 0.3028(2) 0.76949(15) 0.0269(7) Uani 1 1 d . . . . .
H9 H 0.370091 0.330350 0.807390 0.032 Uiso 1 1 calc R U . . .
C10 C 0.2501(2) 0.32778(19) 0.74765(15) 0.0254(6) Uani 1 1 d . . . . .
H10 H 0.218163 0.372530 0.771164 0.030 Uiso 1 1 calc R U . . .
C11 C 0.2050(2) 0.28869(18) 0.69188(14) 0.0215(6) Uani 1 1 d . . . . .
C12 C 0.3972(2) 0.1254(2) 0.64265(15) 0.0266(7) Uani 1 1 d . . . . .
H12 H 0.355398 0.106058 0.603931 0.032 Uiso 1 1 calc R U . . .
C13 C 0.4907(2) 0.1575(2) 0.61373(18) 0.0388(8) Uani 1 1 d . . . . .
H13A H 0.520856 0.110034 0.589154 0.058 Uiso 1 1 calc R U . . .
H13B H 0.533201 0.176919 0.650621 0.058 Uiso 1 1 calc R U . . .
H13C H 0.477798 0.206175 0.582884 0.058 Uiso 1 1 calc R U . . .
C14 C 0.4147(3) 0.0466(2) 0.68822(18) 0.0362(8) Uani 1 1 d . . . . .
H14A H 0.442905 -0.000474 0.662040 0.054 Uiso 1 1 calc R U . . .
H14B H 0.354147 0.026873 0.706345 0.054 Uiso 1 1 calc R U . . .
H14C H 0.458139 0.062795 0.725508 0.054 Uiso 1 1 calc R U . . .
C15 C 0.1082(2) 0.3203(2) 0.66623(16) 0.0291(7) Uani 1 1 d . . . . .
H15 H 0.083598 0.277089 0.632367 0.035 Uiso 1 1 calc R U . . .
C16 C 0.0355(2) 0.3265(2) 0.72239(18) 0.0401(8) Uani 1 1 d . . . . .
H16A H -0.025892 0.345647 0.703187 0.060 Uiso 1 1 calc R U . . .
H16B H 0.057768 0.368602 0.756410 0.060 Uiso 1 1 calc R U . . .
H16C H 0.028139 0.269330 0.743485 0.060 Uiso 1 1 calc R U . . .
C17 C 0.1186(3) 0.4073(2) 0.63019(18) 0.0402(8) Uani 1 1 d . . . . .
H17A H 0.056390 0.426277 0.612390 0.060 Uiso 1 1 calc R U . . .
H17B H 0.162561 0.400791 0.592924 0.060 Uiso 1 1 calc R U . . .
H17C H 0.143676 0.450862 0.662091 0.060 Uiso 1 1 calc R U . . .
C18 C 0.1855(2) 0.23223(18) 0.38730(13) 0.0203(6) Uani 1 1 d . . . . .
C19 C 0.1388(2) 0.31022(18) 0.36972(14) 0.0211(6) Uani 1 1 d . . . . .
C20 C 0.1490(2) 0.34297(19) 0.30478(14) 0.0248(6) Uani 1 1 d . . . . .
H20 H 0.117217 0.395212 0.292073 0.030 Uiso 1 1 calc R U . . .
C21 C 0.2050(2) 0.3004(2) 0.25823(15) 0.0276(7) Uani 1 1 d . . . . .
H21 H 0.210763 0.323062 0.213915 0.033 Uiso 1 1 calc R U . . .
C22 C 0.2524(2) 0.22499(19) 0.27697(15) 0.0245(6) Uani 1 1 d . . . . .
H22 H 0.291766 0.196953 0.245376 0.029 Uiso 1 1 calc R U . . .
C23 C 0.2436(2) 0.18913(18) 0.34100(14) 0.0207(6) Uani 1 1 d . . . . .
C24 C 0.0801(2) 0.35980(19) 0.42041(14) 0.0253(6) Uani 1 1 d . . . . .
H24 H 0.085907 0.328042 0.464341 0.030 Uiso 1 1 calc R U . . .
C25 C 0.1184(2) 0.4511(2) 0.43209(17) 0.0342(8) Uani 1 1 d . . . . .
H25A H 0.080836 0.480293 0.466384 0.051 Uiso 1 1 calc R U . . .
H25B H 0.114073 0.484108 0.389824 0.051 Uiso 1 1 calc R U . . .
H25C H 0.185006 0.447858 0.447597 0.051 Uiso 1 1 calc R U . . .
C26 C -0.0253(2) 0.3621(2) 0.40023(17) 0.0347(8) Uani 1 1 d . . . . .
H26A H -0.060530 0.393221 0.434760 0.052 Uiso 1 1 calc R U . . .
H26B H -0.049462 0.302480 0.396126 0.052 Uiso 1 1 calc R U . . .
H26C H -0.033454 0.392064 0.356839 0.052 Uiso 1 1 calc R U . . .
C27 C 0.2998(2) 0.10889(19) 0.36264(15) 0.0249(6) Uani 1 1 d . . . . .
H27 H 0.263123 0.079015 0.398479 0.030 Uiso 1 1 calc R U . . .
C28 C 0.3141(2) 0.0435(2) 0.30624(16) 0.0316(7) Uani 1 1 d . . . . .
H28A H 0.344508 -0.008994 0.324742 0.047 Uiso 1 1 calc R U . . .
H28B H 0.354758 0.069143 0.272053 0.047 Uiso 1 1 calc R U . . .
H28C H 0.252343 0.028250 0.285580 0.047 Uiso 1 1 calc R U . . .
C29 C 0.3960(2) 0.1358(2) 0.39423(17) 0.0361(8) Uani 1 1 d . . . . .
H29A H 0.429899 0.083983 0.410656 0.054 Uiso 1 1 calc R U . . .
H29B H 0.385610 0.175577 0.431993 0.054 Uiso 1 1 calc R U . . .
H29C H 0.433968 0.165137 0.360222 0.054 Uiso 1 1 calc R U . . .
O1 O 0.3934(11) 0.5934(5) 0.5540(8) 0.0443(16) Uani 0.708(13) 1 d D U P A 1
C30 C 0.3132(9) 0.5632(5) 0.5925(5) 0.0498(19) Uani 0.708(13) 1 d D U P A 1
H30A H 0.326286 0.505156 0.612269 0.060 Uiso 0.708(13) 1 calc R U P A 1
H30B H 0.254921 0.559757 0.563580 0.060 Uiso 0.708(13) 1 calc R U P A 1
C31 C 0.3026(7) 0.6303(5) 0.6467(5) 0.0507(18) Uani 0.708(13) 1 d D U P A 1
H31A H 0.348542 0.620784 0.684619 0.061 Uiso 0.708(13) 1 calc R U P A 1
H31B H 0.237210 0.631099 0.664090 0.061 Uiso 0.708(13) 1 calc R U P A 1
C32 C 0.3248(6) 0.7135(4) 0.6077(4) 0.0506(17) Uani 0.708(13) 1 d D U P A 1
H32A H 0.271214 0.730597 0.577290 0.061 Uiso 0.708(13) 1 calc R U P A 1
H32B H 0.340690 0.762326 0.638578 0.061 Uiso 0.708(13) 1 calc R U P A 1
C33 C 0.4110(5) 0.6846(5) 0.5683(4) 0.0438(17) Uani 0.708(13) 1 d D U P A 1
H33A H 0.416013 0.718358 0.525946 0.053 Uiso 0.708(13) 1 calc R U P A 1
H33B H 0.470406 0.692174 0.595492 0.053 Uiso 0.708(13) 1 calc R U P A 1
O1B O 0.396(3) 0.5889(12) 0.5595(19) 0.041(2) Uani 0.292(13) 1 d D U P A 2
C30B C 0.321(2) 0.5640(11) 0.6053(13) 0.047(3) Uani 0.292(13) 1 d D U P A 2
H30C H 0.345639 0.520929 0.638544 0.056 Uiso 0.292(13) 1 calc R U P A 2
H30D H 0.266807 0.537823 0.579884 0.056 Uiso 0.292(13) 1 calc R U P A 2
C31B C 0.2908(17) 0.6450(12) 0.6401(13) 0.051(3) Uani 0.292(13) 1 d D U P A 2
H31C H 0.287957 0.635761 0.689404 0.061 Uiso 0.292(13) 1 calc R U P A 2
H31D H 0.227633 0.664377 0.622907 0.061 Uiso 0.292(13) 1 calc R U P A 2
C32B C 0.3671(14) 0.7112(10) 0.6235(8) 0.051(2) Uani 0.292(13) 1 d D U P A 2
H32C H 0.422083 0.707277 0.655430 0.062 Uiso 0.292(13) 1 calc R U P A 2
H32D H 0.341585 0.771234 0.623749 0.062 Uiso 0.292(13) 1 calc R U P A 2
C33B C 0.3940(16) 0.6832(13) 0.5524(8) 0.049(3) Uani 0.292(13) 1 d D U P A 2
H33C H 0.345800 0.702146 0.518242 0.058 Uiso 0.292(13) 1 calc R U P A 2
H33D H 0.457043 0.706179 0.540305 0.058 Uiso 0.292(13) 1 calc R U P A 2
O2 O 0.42423(18) 0.52570(16) 0.39255(11) 0.0403(6) Uani 1 1 d . . . . .
C34 C 0.3719(3) 0.4622(3) 0.35309(18) 0.0454(9) Uani 1 1 d . . . . .
H34A H 0.305894 0.482018 0.343859 0.054 Uiso 1 1 calc R U . . .
H34B H 0.370156 0.405544 0.376800 0.054 Uiso 1 1 calc R U . . .
C35 C 0.4255(3) 0.4549(3) 0.28907(18) 0.0432(9) Uani 1 1 d . . . . .
H35A H 0.383053 0.437075 0.250962 0.052 Uiso 1 1 calc R U . . .
H35B H 0.478308 0.412602 0.293808 0.052 Uiso 1 1 calc R U . . .
C36 C 0.4628(3) 0.5466(3) 0.2791(2) 0.0594(12) Uani 1 1 d . . . . .
H36A H 0.530889 0.545400 0.267581 0.071 Uiso 1 1 calc R U . . .
H36B H 0.426696 0.576341 0.242261 0.071 Uiso 1 1 calc R U . . .
C37 C 0.4495(3) 0.5924(3) 0.3447(2) 0.0544(11) Uani 1 1 d . . . . .
H37A H 0.508999 0.622026 0.359474 0.065 Uiso 1 1 calc R U . . .
H37B H 0.398294 0.636405 0.340298 0.065 Uiso 1 1 calc R U . . .
C38 C 0.8154(6) 0.2967(5) 0.5808(4) 0.0594(19) Uani 0.705(6) 1 d D U P B 1
H38A H 0.842223 0.334215 0.616429 0.089 Uiso 0.705(6) 1 calc R U P B 1
H38B H 0.746935 0.289857 0.587075 0.089 Uiso 0.705(6) 1 calc R U P B 1
H38C H 0.826307 0.323130 0.536686 0.089 Uiso 0.705(6) 1 calc R U P B 1
C39 C 0.8623(11) 0.2097(5) 0.5842(7) 0.062(2) Uani 0.705(6) 1 d D U P B 1
H39A H 0.850856 0.183851 0.629022 0.075 Uiso 0.705(6) 1 calc R U P B 1
H39B H 0.931795 0.217921 0.580483 0.075 Uiso 0.705(6) 1 calc R U P B 1
C40 C 0.8287(4) 0.1448(4) 0.5296(3) 0.0568(15) Uani 0.705(6) 1 d D U P B 1
H40A H 0.838267 0.171061 0.484727 0.068 Uiso 0.705(6) 1 calc R U P B 1
H40B H 0.868737 0.091887 0.532893 0.068 Uiso 0.705(6) 1 calc R U P B 1
C41 C 0.7267(4) 0.1189(4) 0.5348(3) 0.0541(15) Uani 0.705(6) 1 d D U P B 1
H41A H 0.686903 0.171996 0.532358 0.065 Uiso 0.705(6) 1 calc R U P B 1
H41B H 0.717504 0.091957 0.579556 0.065 Uiso 0.705(6) 1 calc R U P B 1
C42 C 0.6926(8) 0.0562(9) 0.4809(5) 0.060(2) Uani 0.705(6) 1 d D U P B 1
H42A H 0.623083 0.052197 0.481363 0.090 Uiso 0.705(6) 1 calc R U P B 1
H42B H 0.720257 -0.001357 0.489599 0.090 Uiso 0.705(6) 1 calc R U P B 1
H42C H 0.712281 0.077071 0.436652 0.090 Uiso 0.705(6) 1 calc R U P B 1
C38B C 0.8595(17) 0.2900(13) 0.5671(14) 0.084(5) Uani 0.295(6) 1 d D U P B 2
H38D H 0.899586 0.328428 0.595094 0.126 Uiso 0.295(6) 1 calc R U P B 2
H38E H 0.793631 0.310738 0.567148 0.126 Uiso 0.295(6) 1 calc R U P B 2
H38F H 0.882348 0.290012 0.520766 0.126 Uiso 0.295(6) 1 calc R U P B 2
C39B C 0.864(3) 0.1996(13) 0.5948(16) 0.060(3) Uani 0.295(6) 1 d D U P B 2
H39C H 0.860663 0.202566 0.644551 0.072 Uiso 0.295(6) 1 calc R U P B 2
H39D H 0.926120 0.173712 0.583700 0.072 Uiso 0.295(6) 1 calc R U P B 2
C40B C 0.7843(11) 0.1396(10) 0.5678(6) 0.060(2) Uani 0.295(6) 1 d D U P B 2
H40C H 0.788871 0.083128 0.591709 0.072 Uiso 0.295(6) 1 calc R U P B 2
H40D H 0.722165 0.165893 0.578395 0.072 Uiso 0.295(6) 1 calc R U P B 2
C41B C 0.7873(10) 0.1235(11) 0.4937(7) 0.062(3) Uani 0.295(6) 1 d D U P B 2
H41C H 0.849953 0.097930 0.483533 0.074 Uiso 0.295(6) 1 calc R U P B 2
H41D H 0.783110 0.180345 0.470260 0.074 Uiso 0.295(6) 1 calc R U P B 2
C42B C 0.711(2) 0.065(2) 0.4643(12) 0.072(6) Uani 0.295(6) 1 d D U P B 2
H42D H 0.740320 0.011301 0.447860 0.108 Uiso 0.295(6) 1 calc R U P B 2
H42E H 0.678387 0.094746 0.426689 0.108 Uiso 0.295(6) 1 calc R U P B 2
H42F H 0.665480 0.050824 0.499078 0.108 Uiso 0.295(6) 1 calc R U P B 2


_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.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016).  Three  
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2016) then corrected for absorption by integration using 
SAINT/SADABS v2014/2 (Bruker, 2016) to sort, merge, and scale the combined 
data.  No decay correction was applied.    
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.1040
0.00 -1.00 0.00 0.1210
1.00 1.00 1.00 0.2920
-1.00 -1.00 -1.00 0.1780
0.00 1.00 1.00 0.1780
0.00 -1.00 -1.00 0.2010
1.00 -1.00 0.00 0.2300
-1.00 1.00 0.00 0.2240
1.00 -1.00 -1.00 0.2500
0.00 0.00 -1.00 0.2580
0.00 1.00 -1.00 0.2320
-1.00 0.00 -1.00 0.2120
1.00 0.00 -2.00 0.2750
-2.00 1.00 0.00 0.2490
-1.00 -1.00 2.00 0.2910
-2.00 -2.00 1.00 0.2470
0.00 -2.00 1.00 0.1020
-2.00 0.00 -1.00 0.2170
-2.00 -1.00 -1.00 0.1870
1.00 2.00 0.00 0.2240
1.00 -2.00 1.00 0.1850
1.00 2.00 1.00 0.2270
0.00 2.00 1.00 0.1350
-1.00 -1.00 -2.00 0.1910
1.00 -2.00 -1.00 0.1990
-1.00 2.00 1.00 0.1920
1.00 -1.00 -2.00 0.2590

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
Ni1 N1 1.646(3) . ?
Ni1 N4 1.900(2) . ?
Ni1 N3 1.906(2) . ?
Ca1 N2 2.299(3) . ?
Ca1 N2 2.299(3) 3_666 ?
Ca1 O1B 2.346(12) 3_666 ?
Ca1 O1B 2.346(12) . ?
Ca1 O1 2.352(6) 3_666 ?
Ca1 O1 2.352(6) . ?
Ca1 O2 2.391(2) . ?
Ca1 O2 2.391(2) 3_666 ?
N1 N2 1.163(4) . ?
N3 C2 1.318(4) . ?
N3 C6 1.436(4) . ?
N4 C4 1.331(4) . ?
N4 C18 1.433(3) . ?
C1 C2 1.510(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.403(4) . ?
C3 C4 1.400(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.509(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.408(4) . ?
C6 C7 1.409(4) . ?
C7 C8 1.395(4) . ?
C7 C12 1.513(4) . ?
C8 C9 1.384(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(4) . ?
C10 H10 0.9500 . ?
C11 C15 1.521(4) . ?
C12 C14 1.527(4) . ?
C12 C13 1.530(5) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.525(5) . ?
C15 C16 1.533(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.406(4) . ?
C18 C23 1.410(4) . ?
C19 C20 1.393(4) . ?
C19 C24 1.521(4) . ?
C20 C21 1.391(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.392(4) . ?
C22 H22 0.9500 . ?
C23 C27 1.520(4) . ?
C24 C25 1.519(4) . ?
C24 C26 1.526(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.520(4) . ?
C27 C29 1.534(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O1 C33 1.450(7) . ?
O1 C30 1.453(6) . ?
C30 C31 1.499(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.530(8) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.525(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O1B C30B 1.453(8) . ?
O1B C33B 1.456(10) . ?
C30B C31B 1.491(10) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C31B C32B 1.520(11) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C32B C33B 1.529(10) . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
C33B H33C 0.9900 . ?
C33B H33D 0.9900 . ?
O2 C34 1.441(4) . ?
O2 C37 1.448(4) . ?
C34 C35 1.496(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.519(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.495(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.492(11) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.537(10) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.494(7) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.510(9) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C38B C39B 1.494(13) . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
C39B C40B 1.537(13) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C40B C41B 1.493(10) . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
C41B C42B 1.504(11) . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?

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
N1 Ni1 N4 135.02(11) . . ?
N1 Ni1 N3 129.62(11) . . ?
N4 Ni1 N3 95.32(10) . . ?
N2 Ca1 N2 180.0 . 3_666 ?
N2 Ca1 O1B 90.8(7) . 3_666 ?
N2 Ca1 O1B 89.2(7) 3_666 3_666 ?
N2 Ca1 O1B 89.2(7) . . ?
N2 Ca1 O1B 90.8(7) 3_666 . ?
O1B Ca1 O1B 180.0 3_666 . ?
N2 Ca1 O1 89.5(3) . 3_666 ?
N2 Ca1 O1 90.5(3) 3_666 3_666 ?
N2 Ca1 O1 90.5(3) . . ?
N2 Ca1 O1 89.5(3) 3_666 . ?
O1 Ca1 O1 180.0(7) 3_666 . ?
N2 Ca1 O2 89.72(9) . . ?
N2 Ca1 O2 90.28(9) 3_666 . ?
O1B Ca1 O2 85.4(12) 3_666 . ?
O1B Ca1 O2 94.6(12) . . ?
O1 Ca1 O2 88.3(5) 3_666 . ?
O1 Ca1 O2 91.7(5) . . ?
N2 Ca1 O2 90.28(9) . 3_666 ?
N2 Ca1 O2 89.72(9) 3_666 3_666 ?
O1B Ca1 O2 94.6(12) 3_666 3_666 ?
O1B Ca1 O2 85.4(12) . 3_666 ?
O1 Ca1 O2 91.7(5) 3_666 3_666 ?
O1 Ca1 O2 88.3(5) . 3_666 ?
O2 Ca1 O2 180.00(12) . 3_666 ?
N2 N1 Ni1 178.0(3) . . ?
N1 N2 Ca1 169.9(3) . . ?
C2 N3 C6 121.5(2) . . ?
C2 N3 Ni1 126.36(19) . . ?
C6 N3 Ni1 111.79(18) . . ?
C4 N4 C18 119.8(2) . . ?
C4 N4 Ni1 125.61(19) . . ?
C18 N4 Ni1 114.44(18) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N3 C2 C3 122.0(3) . . ?
N3 C2 C1 120.1(3) . . ?
C3 C2 C1 117.9(3) . . ?
C4 C3 C2 128.1(3) . . ?
C4 C3 H3 115.9 . . ?
C2 C3 H3 115.9 . . ?
N4 C4 C3 122.5(3) . . ?
N4 C4 C5 119.6(2) . . ?
C3 C4 C5 117.9(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 120.4(3) . . ?
C11 C6 N3 119.2(2) . . ?
C7 C6 N3 120.0(2) . . ?
C8 C7 C6 118.9(3) . . ?
C8 C7 C12 120.6(3) . . ?
C6 C7 C12 120.5(3) . . ?
C9 C8 C7 121.3(3) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 119.3(3) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C11 121.6(3) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C6 118.5(3) . . ?
C10 C11 C15 120.8(3) . . ?
C6 C11 C15 120.5(3) . . ?
C7 C12 C14 111.1(2) . . ?
C7 C12 C13 112.2(3) . . ?
C14 C12 C13 110.5(3) . . ?
C7 C12 H12 107.6 . . ?
C14 C12 H12 107.6 . . ?
C13 C12 H12 107.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 109.9(3) . . ?
C11 C15 C16 112.6(3) . . ?
C17 C15 C16 111.1(3) . . ?
C11 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C16 C15 H15 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 120.9(3) . . ?
C19 C18 N4 119.2(2) . . ?
C23 C18 N4 119.8(2) . . ?
C20 C19 C18 118.6(3) . . ?
C20 C19 C24 120.0(3) . . ?
C18 C19 C24 121.4(2) . . ?
C21 C20 C19 121.1(3) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C21 C22 C23 121.6(3) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C22 C23 C18 118.3(3) . . ?
C22 C23 C27 121.4(3) . . ?
C18 C23 C27 120.2(2) . . ?
C25 C24 C19 111.6(3) . . ?
C25 C24 C26 110.9(3) . . ?
C19 C24 C26 112.2(2) . . ?
C25 C24 H24 107.3 . . ?
C19 C24 H24 107.3 . . ?
C26 C24 H24 107.3 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C23 113.9(2) . . ?
C28 C27 C29 110.3(3) . . ?
C23 C27 C29 110.1(2) . . ?
C28 C27 H27 107.4 . . ?
C23 C27 H27 107.4 . . ?
C29 C27 H27 107.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C33 O1 C30 109.7(4) . . ?
C33 O1 Ca1 124.8(7) . . ?
C30 O1 Ca1 123.8(6) . . ?
O1 C30 C31 104.4(5) . . ?
O1 C30 H30A 110.9 . . ?
C31 C30 H30A 110.9 . . ?
O1 C30 H30B 110.9 . . ?
C31 C30 H30B 110.9 . . ?
H30A C30 H30B 108.9 . . ?
C30 C31 C32 100.8(6) . . ?
C30 C31 H31A 111.6 . . ?
C32 C31 H31A 111.6 . . ?
C30 C31 H31B 111.6 . . ?
C32 C31 H31B 111.6 . . ?
H31A C31 H31B 109.4 . . ?
C33 C32 C31 101.0(5) . . ?
C33 C32 H32A 111.6 . . ?
C31 C32 H32A 111.6 . . ?
C33 C32 H32B 111.6 . . ?
C31 C32 H32B 111.6 . . ?
H32A C32 H32B 109.4 . . ?
O1 C33 C32 104.3(6) . . ?
O1 C33 H33A 110.9 . . ?
C32 C33 H33A 110.9 . . ?
O1 C33 H33B 110.9 . . ?
C32 C33 H33B 110.9 . . ?
H33A C33 H33B 108.9 . . ?
C30B O1B C33B 108.3(9) . . ?
C30B O1B Ca1 129.1(14) . . ?
C33B O1B Ca1 122.6(13) . . ?
O1B C30B C31B 106.7(8) . . ?
O1B C30B H30C 110.4 . . ?
C31B C30B H30C 110.4 . . ?
O1B C30B H30D 110.4 . . ?
C31B C30B H30D 110.4 . . ?
H30C C30B H30D 108.6 . . ?
C30B C31B C32B 104.3(9) . . ?
C30B C31B H31C 110.9 . . ?
C32B C31B H31C 110.9 . . ?
C30B C31B H31D 110.9 . . ?
C32B C31B H31D 110.9 . . ?
H31C C31B H31D 108.9 . . ?
C31B C32B C33B 101.7(10) . . ?
C31B C32B H32C 111.4 . . ?
C33B C32B H32C 111.4 . . ?
C31B C32B H32D 111.4 . . ?
C33B C32B H32D 111.4 . . ?
H32C C32B H32D 109.3 . . ?
O1B C33B C32B 101.2(12) . . ?
O1B C33B H33C 111.5 . . ?
C32B C33B H33C 111.5 . . ?
O1B C33B H33D 111.5 . . ?
C32B C33B H33D 111.5 . . ?
H33C C33B H33D 109.3 . . ?
C34 O2 C37 104.7(3) . . ?
C34 O2 Ca1 125.6(2) . . ?
C37 O2 Ca1 126.1(2) . . ?
O2 C34 C35 104.5(3) . . ?
O2 C34 H34A 110.9 . . ?
C35 C34 H34A 110.9 . . ?
O2 C34 H34B 110.9 . . ?
C35 C34 H34B 110.9 . . ?
H34A C34 H34B 108.9 . . ?
C34 C35 C36 103.0(3) . . ?
C34 C35 H35A 111.2 . . ?
C36 C35 H35A 111.2 . . ?
C34 C35 H35B 111.2 . . ?
C36 C35 H35B 111.2 . . ?
H35A C35 H35B 109.1 . . ?
C37 C36 C35 105.8(3) . . ?
C37 C36 H36A 110.6 . . ?
C35 C36 H36A 110.6 . . ?
C37 C36 H36B 110.6 . . ?
C35 C36 H36B 110.6 . . ?
H36A C36 H36B 108.7 . . ?
O2 C37 C36 106.0(3) . . ?
O2 C37 H37A 110.5 . . ?
C36 C37 H37A 110.5 . . ?
O2 C37 H37B 110.5 . . ?
C36 C37 H37B 110.5 . . ?
H37A C37 H37B 108.7 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C38 C39 C40 114.9(6) . . ?
C38 C39 H39A 108.5 . . ?
C40 C39 H39A 108.5 . . ?
C38 C39 H39B 108.5 . . ?
C40 C39 H39B 108.5 . . ?
H39A C39 H39B 107.5 . . ?
C41 C40 C39 113.8(9) . . ?
C41 C40 H40A 108.8 . . ?
C39 C40 H40A 108.8 . . ?
C41 C40 H40B 108.8 . . ?
C39 C40 H40B 108.8 . . ?
H40A C40 H40B 107.7 . . ?
C40 C41 C42 114.2(6) . . ?
C40 C41 H41A 108.7 . . ?
C42 C41 H41A 108.7 . . ?
C40 C41 H41B 108.7 . . ?
C42 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39B C38B H38D 109.5 . . ?
C39B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C39B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C38B C39B C40B 114.0(12) . . ?
C38B C39B H39C 108.8 . . ?
C40B C39B H39C 108.8 . . ?
C38B C39B H39D 108.8 . . ?
C40B C39B H39D 108.8 . . ?
H39C C39B H39D 107.7 . . ?
C41B C40B C39B 113.8(16) . . ?
C41B C40B H40C 108.8 . . ?
C39B C40B H40C 108.8 . . ?
C41B C40B H40D 108.8 . . ?
C39B C40B H40D 108.8 . . ?
H40C C40B H40D 107.7 . . ?
C40B C41B C42B 116.4(13) . . ?
C40B C41B H41C 108.2 . . ?
C42B C41B H41C 108.2 . . ?
C40B C41B H41D 108.2 . . ?
C42B C41B H41D 108.2 . . ?
H41C C41B H41D 107.4 . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

_refine_diff_density_max         1.741
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.071

