Oxidative C(sp3)-H bond cleavage, C-C and C[double bond, length as m-dash]C coupling at a boron center with O2 as the oxidant mediated by platinum(II)
S. Pal; P. Y. Zavalij; A. N. Vedernikov; Chem.Commun. 50 (2014) 5376–; doi:10.1039/C3CC47445C

data_7112653
_publ_section_title
;
 Oxidative C(sp3)-H bond cleavage, C-C and C[double bond, length as
 m-dash]C coupling at a boron center with O2 as the oxidant mediated by
 platinum(II)
;
_journal_name_full               Chem.Commun.
_journal_page_first              5376
_journal_paper_doi               10.1039/C3CC47445C
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '2(C44 H68 B2 N4 Na2 O8 Pt2), (C4 H8 O)'
_chemical_formula_sum            'C23 H36 B N2 Na O4.25 Pt'
_chemical_formula_weight         637.43
_chemical_name_common            Pt-complex
_chemical_name_systematic
;
Pt-complex
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2012 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 116.3130(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5793(11)
_cell_length_b                   17.8585(11)
_cell_length_c                   17.6641(11)
_cell_measurement_reflns_used    17591
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.3
_cell_volume                     4970.9(5)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2012'
_computing_structure_refinement  'ShelXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0334971
_diffrn_orient_matrix_UB_12      0.0422037
_diffrn_orient_matrix_UB_13      0.0369331
_diffrn_orient_matrix_UB_21      0.0076854
_diffrn_orient_matrix_UB_22      0.0218001
_diffrn_orient_matrix_UB_23      -0.0483025
_diffrn_orient_matrix_UB_31      -0.0533480
_diffrn_orient_matrix_UB_32      0.0296487
_diffrn_orient_matrix_UB_33      -0.0170694
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60095
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    5.695
_exptl_absorpt_correction_T_max  0.505
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_id                'Vedern-Shrin BBNPtMeOMe_MeOH_OxPdt'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.259
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         14457
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+11.9000P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12135
_reflns_number_total             14457
_reflns_threshold_expression     'I > 2\s(I)'
_iucr_refine_instructions_details 'See _shelx_res_file'
_cod_data_source_file            c3cc47445c.txt
_cod_data_source_block           2369
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7112653
_shelx_estimated_absorpt_t_min   0.411
_shelx_estimated_absorpt_t_max   0.548