Expanding the allyl analogy: accessing η<sup>3</sup>-P,B,P diphosphinoborane complexes of group 10.
Drover, Marcus W.; Peters, Jonas C.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3733–3738; doi:10.1039/c8dt00058a

data_7045541
_publ_section_title
;
 Expanding the allyl analogy: accessing \h<sup>3</sup>-P,B,P
 diphosphinoborane complexes of group 10.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3733
_journal_page_last               3738
_journal_paper_doi               10.1039/c8dt00058a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C66.88 H64.65 B2 I1.12 P4 Pt, C4 H10 O'
_chemical_formula_sum            'C70.88 H74.65 B2 I1.12 O P4 Pt'
_chemical_formula_weight         1424.94
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-23
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-23 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.522(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3295(6)
_cell_length_b                   19.2099(9)
_cell_length_c                   27.5709(13)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.050
_cell_measurement_theta_min      2.463
_cell_volume                     6509.8(5)
_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, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker AXS D8 Venture Kappa'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            189791
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.064
_diffrn_reflns_theta_min         1.482
_exptl_absorpt_coefficient_mu    2.826
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0563 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.8950.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             2861
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.481
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         17777
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+14.7365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14977
_reflns_number_total             17777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00058a2.cif
_cod_data_source_block           a17024_final
_cod_depositor_comments
'Adding full bibliography for 7045536--7045541.cif.'
_cod_database_code               7045541
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.728
_shelx_estimated_absorpt_t_min   0.602
_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. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
3. Others
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=1-FVAR(1)
 Sof(I2)=FVAR(1)
 Fixed Sof: I1(0.56255) C1(0.43745) H1A(0.43745) H1B(0.43745) H1C(0.43745)
4.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C70(H70A,H70B)
4.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C24(H24), C22(H22), C26(H26), C16(H16), C31(H31), C20(H20),
 C19(H19), C59(H59), C29(H29), C58(H58), C53(H53), C37(H37), C10(H10), C23(H23),
  C43(H43), C62(H62), C50(H50), C41(H41), C52(H52), C51(H51), C44(H44),
 C55(H55), C25(H25), C12(H12), C11(H11), C64(H64), C14(H14), C5(H5), C40(H40),
 C4(H4), C47(H47), C13(H13), C38(H38), C39(H39), C46(H46), C8(H8), C45(H45),
 C18(H18), C57(H57), C56(H56), C6(H6), C7(H7), C17(H17)
4.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C67(H67A,H67B,H67C), C66(H66A,H66B,
 H66C), C35(H35A,H35B,H35C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C72(H72A,
 H72B,H72C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'