The phosphinoboration of acyl chlorides.
Murphy, Maia C.; Trofimova, Alina; LaFortune, James H. W.; Vogels, Christopher M.; Geier, Stephen J.; Binder, Justin F.; Macdonald, Charles L. B.; Stephan, Douglas W.; Westcott, Stephen A.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5092–5099; doi:10.1039/d0dt00579g

data_7703696
_publ_section_title
;
 The phosphinoboration of acyl chlorides.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5092
_journal_page_last               5099
_journal_paper_doi               10.1039/d0dt00579g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C46 H44 B O3 P2 Rh'
_chemical_formula_sum            'C46 H44 B O3 P2 Rh'
_chemical_formula_weight         820.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-15 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.508(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3384(5)
_cell_length_b                   17.0645(8)
_cell_length_c                   11.1586(6)
_cell_measurement_reflns_used    9382
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      28.780
_cell_measurement_theta_min      2.973
_cell_volume                     1967.91(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            96896
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.788
_diffrn_reflns_theta_min         2.972
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0638 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.9071. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 4377 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.047(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         10161
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0159P)^2^+0.8002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                9559
_reflns_number_total             10161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00579g2.cif
_cod_data_source_block           rh6
_cod_depositor_comments
'Adding full bibliography for 7703695--7703698.cif.'
_cod_database_code               7703696
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C21(H21), C22(H22), C33(H33), C4(H4), C23(H23), C37(H37), C7(H7),
 C30(H30), C31(H31), C19(H19), C28(H28), C25(H25), C29(H29), C35(H35), C34(H34),
  C36(H36), C5(H5), C27(H27), C24(H24), C6(H6), C17(H17), C15(H15), C18(H18),
 C16(H16), C48(H48), C41(H41), C40(H40), C46(H46), C43(H43), C45(H45), C44(H44)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              61958
_olex2_submission_special_instructions 'No special instructions were received'