# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_CuBr2_LT
_database_code_depnum_ccdc_archive 'CCDC 1580083'
_audit_update_record             
;
2017-10-15 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
#===============================================================================
# 5. CHEMICAL DATA

_chemical_formula_moiety         'C4 H4 Br2 Cu N4 O2 Pt'
_chemical_formula_sum            'C4 H4 Br2 Cu N4 O2 Pt'
_chemical_formula_weight         558.53
#=============================================================
# 6. CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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


#------------------------------------------------
_cell_length_a                   6.3039(6)
_cell_length_b                   14.2946(13)
_cell_length_c                   6.5640(6)
_cell_angle_alpha                90
_cell_angle_beta                 110.207(2)
_cell_angle_gamma                90
_cell_volume                     555.09(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    135(2)

_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      33.24

_exptl_crystal_description       octahedral
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.048

_exptl_crystal_density_diffrn    3.336
_exptl_crystal_density_meas      ?
# Non-dispersive F(000): 
_exptl_crystal_F_000             496

_exptl_absorpt_coefficient_mu    21.680
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   '(Sheldrick , 1996)'
_shelx_estimated_absorpt_T_min   0.145
_shelx_estimated_absorpt_T_max   0.423
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_T_max  0.348

#=============================================================================
# 7. EXPERIMENTAL DATA

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'φ and ω scans'
_diffrn_ambient_temperature      135(2)
_diffrn_reflns_number            2208
_diffrn_reflns_av_R_equivalents  ?

_diffrn_reflns_theta_min         2.850
_diffrn_reflns_theta_max         33.240
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       10


#==========================================================================
# 8. REFINEMENT DATA


# The values actually used during refinement 
# The I/u(I) cutoff below was used for refinement as 
# well as the _gt R-factors: 
_reflns_number_total             2208
_reflns_number_gt                1665
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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.

 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0165P)²+0.0234P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00104(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2208
_refine_ls_number_parameters     79
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0141
_refine_ls_wR_factor_ref         0.0338
_refine_ls_wR_factor_gt          0.0309
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_diff_density_max         1.160
_refine_diff_density_min         -0.985
#========================================================== 
# 9. General computing 

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'


#===================================================================
# 10.  ATOMIC COORDINATES AND THERMAL PARAMETERS

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Pt1 Pt 0.0000 0.5000 0.0000 0.00638(4) Uani 1 2 d S . P . .
O1 O 0.2190(6) 0.2500 0.6756(6) 0.0267(8) Uani 1 2 d DS T P . .
Br1 Br -0.23341(5) 0.50704(2) 0.23567(5) 0.01549(5) Uani 1 1 d . . . . .
Cu1 Cu 0.50467(12) 0.2500 0.49653(11) 0.00749(6) Uani 1 2 d S T P . .
N1 N 0.6822(5) 0.34743(16) 0.7006(5) 0.0124(6) Uani 1 1 d . . . . .
H1 H 0.282(9) 0.289(2) 0.792(5) 0.076(19) Uiso 1 1 d D . . . .
C1 C 0.7962(6) 0.40212(18) 0.8121(5) 0.0105(6) Uani 1 1 d . . . . .
N2 N 0.3142(5) 0.34715(16) 0.3020(5) 0.0121(6) Uani 1 1 d . . . . .
H2 H 0.910(5) 0.2500 0.413(8) 0.050(19) Uiso 1 2 d DS . P . .
O2 O 0.7682(6) 0.2500 0.3243(6) 0.0328(9) Uani 1 2 d DS T P . .
C2 C 0.1977(5) 0.40183(18) 0.1913(5) 0.0099(6) 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
Pt1 C2 2.005(3) . ?
Pt1 C2 2.005(3) 3_565 ?
Pt1 C1 2.009(3) 3_666 ?
Pt1 C1 2.009(3) 1_454 ?
Pt1 Br1 2.4780(3) . ?
Pt1 Br1 2.4780(3) 3_565 ?
O1 Cu1 2.467(3) . ?
O1 O2 2.978(5) 1_455 ?
O1 H1 0.918(19) . ?
Br1 O1 3.5175(6) 2_556 ?
Br1 Br1 3.6997(7) 3_566 ?
Br1 Br1 3.7048(8) 3_465 ?
Br1 O2 3.7196(6) 1_455 ?
Cu1 N2 1.985(3) 4_565 ?
Cu1 N2 1.985(3) . ?
Cu1 N1 1.988(3) 4_565 ?
Cu1 N1 1.988(3) . ?
Cu1 O2 2.309(3) . ?
N1 C1 1.140(4) . ?
C1 Pt1 2.009(3) 1_656 ?
N2 C2 1.144(4) . ?
O2 H2 0.88(2) . ?

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
C2 Pt1 C2 180.0 . 3_565 ?
C2 Pt1 C1 88.60(7) . 3_666 ?
C2 Pt1 C1 91.40(7) 3_565 3_666 ?
C2 Pt1 C1 91.40(7) . 1_454 ?
C2 Pt1 C1 88.60(7) 3_565 1_454 ?
C1 Pt1 C1 180.0 3_666 1_454 ?
C2 Pt1 Br1 90.70(7) . . ?
C2 Pt1 Br1 89.30(7) 3_565 . ?
C1 Pt1 Br1 88.86(7) 3_666 . ?
C1 Pt1 Br1 91.14(7) 1_454 . ?
C2 Pt1 Br1 89.30(7) . 3_565 ?
C2 Pt1 Br1 90.70(7) 3_565 3_565 ?
C1 Pt1 Br1 91.14(7) 3_666 3_565 ?
C1 Pt1 Br1 88.86(7) 1_454 3_565 ?
Br1 Pt1 Br1 180.0 . 3_565 ?
Cu1 O1 O2 106.84(13) . 1_455 ?
Cu1 O1 H1 103(4) . . ?
O2 O1 H1 132(3) 1_455 . ?
Pt1 Br1 O1 99.01(5) . 2_556 ?
Pt1 Br1 Br1 97.577(14) . 3_566 ?
O1 Br1 Br1 86.09(6) 2_556 3_566 ?
Pt1 Br1 Br1 92.264(13) . 3_465 ?
O1 Br1 Br1 98.98(6) 2_556 3_465 ?
Br1 Br1 Br1 168.119(13) 3_566 3_465 ?
Pt1 Br1 O2 95.02(5) . 1_455 ?
O1 Br1 O2 161.97(7) 2_556 1_455 ?
Br1 Br1 O2 80.86(6) 3_566 1_455 ?
Br1 Br1 O2 91.70(6) 3_465 1_455 ?
N2 Cu1 N2 88.77(16) 4_565 . ?
N2 Cu1 N1 91.03(7) 4_565 4_565 ?
N2 Cu1 N1 176.59(9) . 4_565 ?
N2 Cu1 N1 176.59(9) 4_565 . ?
N2 Cu1 N1 91.03(7) . . ?
N1 Cu1 N1 88.96(16) 4_565 . ?
N2 Cu1 O2 93.59(9) 4_565 . ?
N2 Cu1 O2 93.59(9) . . ?
N1 Cu1 O2 89.83(9) 4_565 . ?
N1 Cu1 O2 89.83(9) . . ?
N2 Cu1 O1 85.86(9) 4_565 . ?
N2 Cu1 O1 85.86(9) . . ?
N1 Cu1 O1 90.73(8) 4_565 . ?
N1 Cu1 O1 90.73(8) . . ?
O2 Cu1 O1 179.22(13) . . ?
C1 N1 Cu1 175.1(2) . . ?
N1 C1 Pt1 178.0(2) . 1_656 ?
C2 N2 Cu1 177.5(2) . . ?
Cu1 O2 H2 114(4) . . ?
N2 C2 Pt1 178.5(3) . . ?


# start Validation Reply Form
_vrf_PLAT041_CuBr2_LT            
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: One hydrogen was not found. HFIX did not result in realistic hydrogens therefore they were placed not simulated.
;
_vrf_PLAT043_CuBr2_LT            
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       1.00 Check 
RESPONSE: One hydrogen was not found.
;
# end Validation Reply Form
_chemical_name_systematic        
'bis(aqua)tetrakis(μ-2cyano)copper(II) dibromoplatinate(IV)'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Heat-sensitive
_refine_special_details          Twin
