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_1569576
_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         'C102 H90 Na2 O2 P6 Rh2'
_chemical_formula_sum            'C102 H90 Na2 O2 P6 Rh2'
_chemical_formula_weight         1785.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-04 deposited with the CCDC.	2023-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                93.6980(10)
_cell_angle_beta                 91.5350(10)
_cell_angle_gamma                98.4790(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1385(2)
_cell_length_b                   16.5943(2)
_cell_length_c                   20.8960(3)
_cell_measurement_reflns_used    83282
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      32.6880
_cell_measurement_theta_min      2.1200
_cell_volume                     4493.61(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            228372
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.651
_diffrn_reflns_theta_min         2.106
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70999
_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    1.319
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.492
_refine_diff_density_min         -1.653
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         30654
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0739
_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^)+(0.0785P)^2^+26.0119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24033
_reflns_number_total             30654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02292g3.cif
_cod_data_source_block           okabe_rh2_retry_auto
_cod_depositor_comments
'Adding full bibliography for 1569575--1569576.cif.'
_cod_database_code               1569576
_shelx_shelxl_version_number     2017/1
_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. Restrained distances
 C99-C100
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C100 \\sim C99 \\sim O2 \\sim C101 \\sim C102 \\sim C96 \\sim C95 \\sim O1
\\sim C97 \\sim C98: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
Uanis(C100) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C101)
\\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C95) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C95(H95A,H95B), C101(H10A,H10B), C97(H97A,H97B), C99(H99A,H99B)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C25(H25), C28(H28), C29(H29), C15(H15), C4(H4), C31(H31), C51(H51),
 C13(H13), C66(H66), C19(H19), C49(H49), C26(H26), C14(H14), C67(H67), C32(H32),
  C35(H35), C27(H27), C2(H2), C88(H88), C76(H76), C20(H20), C69(H69), C34(H34),
 C75(H75), C90(H90), C37(H37), C33(H33), C58(H58), C60(H60), C82(H82), C63(H63),
  C22(H22), C92(H92), C21(H21), C68(H68), C87(H87), C80(H80), C79(H79),
 C44(H44), C94(H94), C54(H54), C84(H84), C74(H74), C41(H41), C93(H93), C91(H91),
  C78(H78), C81(H81), C56(H56), C11(H11), C72(H72), C62(H62), C57(H57),
 C61(H61), C38(H38), C43(H43), C86(H86), C85(H85), C55(H55), C73(H73), C45(H45),
  C8(H8), C7(H7), C9(H9), C40(H40), C10(H10), C39(H39), C47(H47), C46(H46)
4.c Idealised Me refined as rotating group:
 C98(H98A,H98B,H98C), C96(H96A,H96B,H96C), C102(H10C,H10D,H10E), C100(H10F,
 H10G,H10H)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70472
_shelx_fab_checksum              94477
_olex2_submission_special_instructions 'No special instructions were received'