A dinuclear Rh(-i)/Rh(i) complex bridged by biphilic phosphinine ligands.
Masada, Koichiro; Okabe, Kiyosumi; Kusumoto, Shuhei; Nozaki, Kyoko; Chemical science 14 (2023) 8524–8530; doi:10.1039/d3sc02292g

data_1569575
_publ_section_title
;
 A dinuclear Rh(-i)/Rh(i) complex bridged by biphilic phosphinine ligands.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              8524
_journal_page_last               8530
_journal_paper_doi               10.1039/d3sc02292g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C94 H70 P6 Rh2, C7 H8'
_chemical_formula_sum            'C101 H78 P6 Rh2'
_chemical_formula_weight         1683.27
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-05-04 deposited with the CCDC.	2023-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.453(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4813(3)
_cell_length_b                   19.1877(3)
_cell_length_c                   28.5841(5)
_cell_measurement_reflns_used    40015
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      29.6960
_cell_measurement_theta_min      2.7330
_cell_volume                     8998.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     55.00  81.00   0.50   90.09    --   -1.70  46.00  60.00   52
  2  \w     17.00  57.00   0.50   90.09    --   -1.70  18.00 120.00   80
  3  \w    -19.00   7.00   0.50   90.09    --   -1.70  46.00  60.00   52
  4  \w      9.00  78.00   0.50   90.09    --    2.60  28.00  90.00  138
  5  \w    -58.00  92.00   0.50   90.09    --    2.60   9.00 -30.00  300
  6  \w     44.00  75.00   0.50   90.09    --    2.60  28.00   0.00   62
  7  \w     30.00  92.00   0.50   90.09    --    2.60  37.00-150.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0099126000
_diffrn_orient_matrix_UB_12      -0.0348824000
_diffrn_orient_matrix_UB_13      -0.0053795000
_diffrn_orient_matrix_UB_21      -0.0202960000
_diffrn_orient_matrix_UB_22      0.0039841000
_diffrn_orient_matrix_UB_23      -0.0228588000
_diffrn_orient_matrix_UB_31      0.0368588000
_diffrn_orient_matrix_UB_32      0.0115742000
_diffrn_orient_matrix_UB_33      -0.0083638000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            128571
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.535
_diffrn_reflns_theta_min         2.240
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       plate
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.486
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         22289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0467P)^2^+35.4213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19349
_reflns_number_total             22289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02292g3.cif
_cod_data_source_block           13086_auto
_cod_depositor_comments
'Adding full bibliography for 1569575--1569576.cif.'
_cod_database_code               1569575
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C102H86Li2O2P6Rh2
_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:
 C22(H22), C4(H4), C51(H51), C60(H60), C2(H2), C49(H49), C63(H63), C47(H47),
 C66(H66), C21(H21), C58(H58), C61(H61), C19(H19), C62(H62), C16(H16), C13(H13),
  C15(H15), C14(H14), C43(H43), C35(H35), C37(H37), C69(H69), C88(H88), C7(H7),
 C20(H20), C76(H76), C31(H31), C84(H84), C34(H34), C41(H41), C82(H82), C57(H57),
  C8(H8), C11(H11), C25(H25), C67(H67), C68(H68), C54(H54), C32(H32), C87(H87),
 C90(H90), C46(H46), C44(H44), C80(H80), C9(H9), C75(H75), C72(H72), C38(H38),
 C86(H86), C85(H85), C33(H33), C40(H40), C81(H81), C45(H45), C10(H10), C39(H39),
  C56(H56), C78(H78), C91(H91), C79(H79), C55(H55), C29(H29), C74(H74),
 C94(H94), C73(H73), C92(H92), C93(H93), C26(H26), C28(H28), C27(H27), C97(H97),
  C98(H98), C100(H100), C96(H96), C99(H99)
2.b Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55345
_shelx_fab_checksum              87590
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.440
_oxdiff_exptl_absorpt_empirical_full_min 0.612