A sterically congested 1,2-diphosphino-1'-boryl-ferrocene: synthesis, characterization and coordination to platinum.
Lerayer, Emmanuel; Renaut, Patrice; Roger, Julien; Pirio, Nadine; Cattey, Hélène; Fleurat-Lessard, Paul; Boudjelel, Maxime; Massou, Stéphane; Bouhadir, Ghenwa; Bourissou, Didier; Hierso, Jean-Cyrille; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11191–11195; doi:10.1039/c9dt01921a

data_7700436
_publ_section_title
;
 A sterically congested 1,2-diphosphino-1'-boryl-ferrocene: synthesis,
 characterization and coordination to platinum.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11191
_journal_page_last               11195
_journal_paper_doi               10.1039/c9dt01921a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C60 H65 B Cl2 Fe P2 Pt, C H2 Cl2'
_chemical_formula_sum            'C61 H67 B Cl4 Fe P2 Pt'
_chemical_formula_weight         1265.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2019-06-04 deposited with the CCDC.    2019-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.454(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3692(11)
_cell_length_b                   32.732(3)
_cell_length_c                   16.6670(14)
_cell_measurement_reflns_used    9788
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.79
_cell_volume                     6562.8(10)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '\k-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 Venture triumph Mo'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            57058
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.462
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_exptl_absorpt_coefficient_mu    2.595
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0721 before and 0.0557 after correction. The Ratio of minimum to maximum transmission is 0.9195. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       prism
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.843
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         12046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0293P)^2^+27.7394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9746
_reflns_number_total             12046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01921a2.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
'Adding full bibliography for 7700435--7700436.cif.'
_cod_original_cell_volume        6562.7(10)
_cod_database_code               7700436
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C33(H33), C32(H32), C31(H31), C30(H30), C28(H28), C27(H27),
 C26(H26), C25(H25), C24(H24), C9(H9), C10(H10), C50(H50), C52(H52), C41(H41),
 C43(H43), C7(H7), C5(H5), C3(H3), C22(H22), C21(H21), C20(H20), C19(H19),
 C18(H18), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C54(H54A,H54B,H54C), C47(H47A,H47B,H47C), C45(H45A,H45B,
 H45C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C55(H55A,H55B,H55C),
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              218
_shelx_fab_checksum              28328
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'