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_4124832
_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         'C14 H25 Br N2 Pt'
_chemical_formula_sum            'C14 H25 Br N2 Pt'
_chemical_formula_weight         496.36
_chemical_name_systematic
bromo-dimethyl-(C,N,N'-(2-(((2-(dimethylamino)ethyl)(methyl)amino)methyl)phenyl)platinum
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                94.032(4)
_cell_angle_beta                 101.952(5)
_cell_angle_gamma                103.382(5)
_cell_formula_units_Z            2
_cell_length_a                   7.3874(14)
_cell_length_b                   8.2772(16)
_cell_length_c                   13.402(3)
_cell_measurement_reflns_used    6007
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.485
_cell_measurement_theta_min      2.822
_cell_volume                     773.9(3)
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.603
_diffrn_reflns_theta_min         1.565
_exptl_absorpt_coefficient_mu    11.634
_exptl_absorpt_correction_T_max  0.2203
_exptl_absorpt_correction_T_min  0.1383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0693 before and 0.0303 after correction.
The Ratio of minimum to maximum transmission is 0.6278.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_description       prism
_exptl_crystal_F_000             472
_exptl_crystal_preparation
'Slow evaporation of dichloromethane solution'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.420
_refine_diff_density_min         -2.326
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+1.8258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4481
_reflns_number_total             4742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10993_si_002.cif
_cod_data_source_block           mo_jl134_0m
_cod_database_code               4124832
_shelx_estimated_absorpt_t_max   0.313
_shelx_estimated_absorpt_t_min   0.123
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.023) H1B(0.023) H1C(0.023) H2A(0.023) H2B(0.023) H2C(0.023)
 H4(0.021) H5(0.023) H6(0.02) H7(0.019) H9A(0.017) H9B(0.017) H10A(0.023)
 H10B(0.023) H10C(0.023) H11A(0.015) H11B(0.015) H12A(0.014) H12B(0.014)
 H13A(0.023) H13B(0.023) H13C(0.023) H14A(0.025) H14B(0.025) H14C(0.025)
 Fixed X: H1A(0.3003) H1B(0.2191) H1C(0.1296) H2A(0.1608) H2B(0.3325)
 H2C(0.3343) H4(0.5154) H5(0.7442) H6(0.9883) H7(1) H9A(0.8937) H9B(0.6852)
 H10A(0.5153) H10B(0.7331) H10C(0.5901) H11A(0.9003) H11B(0.9054) H12A(0.8158)
 H12B(0.6366) H13A(0.6466) H13B(0.7992) H13C(0.8149) H14A(0.3933) H14B(0.5564)
 H14C(0.3991)
 Fixed Y: H1A(0.0247) H1B(0.1877) H1C(0.0295) H2A(0.3255) H2B(0.4578)
 H2C(0.433) H4(0.278) H5(0.474) H6(0.668) H7(0.6661) H9A(0.5136) H9B(0.5482)
 H10A(0.3568) H10B(0.3757) H10C(0.1937) H11A(0.2079) H11B(0.2381) H12A(-0.0523)
 H12B(-0.0279) H13A(-0.0025) H13B(-0.0738) H13C(0.123) H14A(-0.1983) H14B(-
 0.2604) H14C(-0.1957)
 Fixed Z: H1A(0.0727) H1B(0.0763) H1C(0.1285) H2A(0.2407) H2B(0.2127)
 H2C(0.3303) H4(0.03) H5(-0.0252) H6(0.0947) H7(0.271) H9A(0.4099) H9B(0.3858)
 H10A(0.4837) H10B(0.5413) H10C(0.5075) H11A(0.4597) H11B(0.3434) H12A(0.3565)
 H12B(0.4003) H13A(0.1014) H13B(0.1769) H13C(0.1859) H14A(0.2708) H14B(0.2287)
 H14C(0.1522)
;
_shelx_res_checksum              49744
_shelx_hkl_checksum              65445
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id EB_2A
_olex2_submission_special_instructions 'No special instructions were received'