Synthesis and characterisation of boranediyl- and diboranediyl-bridged diplatinum A-frame complexes.
Brunecker, Carina; Arrowsmith, Merle; Müssig, Jonas H; Böhnke, Julian; Stoy, Andreas; Heß, Merlin; Hofmann, Alexander; Lenczyk, Carsten; Lichtenberg, Crispin; Ramler, Jacqueline; Rempel, Anna; Braunschweig, Holger; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3506–3515; doi:10.1039/d0dt03855e

data_7706367
_publ_section_title
;
 Synthesis and characterisation of boranediyl- and diboranediyl-bridged
 diplatinum A-frame complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3506
_journal_page_last               3515
_journal_paper_doi               10.1039/d0dt03855e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C20 H41 B Br2 Cl2 P4 Pt2'
_chemical_formula_sum            'C20 H41 B Br2 Cl2 P4 Pt2'
_chemical_formula_weight         1037.12
_chemical_name_systematic        4-Br(Mes)
_chemical_properties_physical
'Air-sensitive,Moisture-sensitive,Heat-sensitive,slowly decomposes in solution'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-11-06 deposited with the CCDC.	2021-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.731(4)
_cell_length_b                   15.170(4)
_cell_length_c                   19.590(9)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.48
_cell_volume                     3189(2)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            177701
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.722
_diffrn_reflns_theta_min         2.164
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    11.647
_exptl_absorpt_correction_T_max  0.2458
_exptl_absorpt_correction_T_min  0.1604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/pentane'
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 2880 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0010(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0120
_refine_ls_R_factor_gt           0.0115
_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^)+(0.0073P)^2^+3.5263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0257
_refine_ls_wR_factor_ref         0.0258
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6663
_reflns_number_total             6760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03855e2.cif
_cod_data_source_block           test_a_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7706356--7706368.cif.'
_cod_database_code               7706367
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.148
_shelx_estimated_absorpt_t_max   0.372
_shelx_res_checksum              96929