Exclusive Csp(3)-Csp(3) vs Csp(2)-Csp(3) Reductive Elimination from Pt(IV) Governed by Ligand Constraints.
Bowes, Eric G.; Pal, Shrinwantu; Love, Jennifer A.; Journal of the American Chemical Society 137 (2015) 16004–16007; doi:10.1021/jacs.5b10993

data_4124833
_publ_section_title
;
 Exclusive Csp(3)-Csp(3) vs Csp(2)-Csp(3) Reductive Elimination from
 Pt(IV) Governed by Ligand Constraints.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16004
_journal_page_last               16007
_journal_paper_doi               10.1021/jacs.5b10993
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C11 H16 Br N Pt S'
_chemical_formula_sum            'C11 H16 Br N Pt S'
_chemical_formula_weight         469.31
_chemical_name_systematic
bromine-(dimethylsufide)-(C,N-(3-methyl-2-((methylimino)methyl)phenyl)platinum
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.915(3)
_cell_length_b                   25.896(5)
_cell_length_c                   11.227(3)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.213
_cell_measurement_theta_min      2.282
_cell_volume                     5208.5(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26043
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.196
_diffrn_reflns_theta_min         2.281
_exptl_absorpt_coefficient_mu    13.974
_exptl_absorpt_correction_T_max  0.1069
_exptl_absorpt_correction_T_min  0.0690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0981 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.6452.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.394
_exptl_crystal_description       prism
_exptl_crystal_F_000             3488
_exptl_crystal_preparation
'Crystals grown from a saturated Et2O solution'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 1642 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3522
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0106
_refine_ls_R_factor_gt           0.0104
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0248
_refine_ls_wR_factor_ref         0.0249
_reflns_Friedel_coverage         0.902
_reflns_friedel_fraction_full    0.993
_reflns_friedel_fraction_max     0.989
_reflns_number_gt                3500
_reflns_number_total             3522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10993_si_002.cif
_cod_data_source_block           jl159_2_fdd2_a
_cod_original_cell_volume        5208.4(18)
_cod_database_code               4124833
_shelx_estimated_absorpt_t_max   0.213
_shelx_estimated_absorpt_t_min   0.098
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              97890
_shelx_hkl_checksum              72259
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id EB_3D
_olex2_submission_special_instructions 'No special instructions were received'