Sodium phosphaethynolate as P-source for the synthesis of molecular rhodium phosphides: an exploratory study.
Li, Zhongshu; Borger, Jaap E.; Gianetti, Thomas L.; Müller, Fabian; Pribanic, Bruno; Coburger, Peter; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16718–16726; doi:10.1039/d5dt02274f

data_7719509
_publ_section_title
;
 Sodium phosphaethynolate as P-source for the synthesis of molecular
 rhodium phosphides: an exploratory study.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16718
_journal_page_last               16726
_journal_paper_doi               10.1039/d5dt02274f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C110 H84 O2 P8 Rh4, C4 H8 O'
_chemical_formula_sum            'C114 H93 O3 P8 Rh4'
_chemical_formula_weight         2170.28
_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             2019-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-01-09 deposited with the CCDC.	2025-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                88.720(2)
_cell_angle_beta                 74.986(2)
_cell_angle_gamma                76.727(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5881(3)
_cell_length_b                   15.3992(4)
_cell_length_c                   23.9098(4)
_cell_measurement_reflns_used    55661
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.6000
_cell_measurement_theta_min      2.1750
_cell_volume                     5045.3(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -100.00  -2.00   1.00    7.50    --  -30.40 -77.00 150.00   98
  2  \w   -100.00  -2.00   1.00    7.50    --  -30.40 -77.00-120.00   98
  3  \w    -68.00  42.00   1.00    7.50    --  -30.40  19.00 120.00  110
  4  \w   -100.00  -2.00   1.00    7.50    --  -30.40 -77.00  60.00   98
  5  \w   -101.00  -8.00   1.00    7.50    --  -30.40 -38.00 120.00   93
  6  \w   -100.00  -2.00   1.00    7.50    --  -30.40 -77.00 -30.00   98
  7  \w     -5.00  84.00   1.00    7.50    --   30.87-123.00  90.00   89
  8  \w    -25.00  71.00   1.00    7.50    --   30.87 -99.00-180.00   96
  9  \w    -25.00  71.00   1.00    7.50    --   30.87 -99.00 -90.00   96
 10  \w     32.00 105.00   1.00    7.50    --   30.87-179.00  60.00   73
 11  \w    -40.00 102.00   1.00    7.50    --   30.87   0.00 150.00  142
 12  \w   -105.00 -34.00   1.00    7.50    --  -30.40-179.00  90.00   71
 13  \w   -100.00  -2.00   1.00    7.50    --  -30.40 -77.00-180.00   98
 14  \w   -105.00 -34.00   1.00    7.50    --  -30.40-179.00   0.00   71
 15  \w    -99.00 -12.00   1.00    7.50    --  -30.40 -57.00-120.00   87
 16  \w    -99.00 -12.00   1.00    7.50    --  -30.40 -57.00  90.00   87
 17  \w   -101.00  -8.00   1.00    7.50    --  -30.40 -38.00 -90.00   93
 18  \w    -40.00  53.00   1.00    7.50    --   30.87 -38.00-180.00   93
 19  \w     -7.00 103.00   1.00    7.50    --   30.87  19.00 -30.00  110
 20  \w     34.00 105.00   1.00    7.50    --   30.87 179.00 120.00   71
 21  \w   -102.00  41.00   1.00    7.50    --  -30.40   0.00-150.00  143
 22  \w   -102.00  41.00   1.00    7.50    --  -30.40   0.00-120.00  143
 23  \w   -102.00  41.00   1.00    7.50    --  -30.40   0.00 -90.00  143
 24  \w   -102.00  41.00   1.00    7.50    --  -30.40   0.00 -60.00  143
 25  \w   -102.00  41.00   1.00    7.50    --  -30.40   0.00-180.00  143
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0295307000
_diffrn_orient_matrix_UB_12      0.0104234000
_diffrn_orient_matrix_UB_13      -0.0196960000
_diffrn_orient_matrix_UB_21      -0.0413093000
_diffrn_orient_matrix_UB_22      0.0166996000
_diffrn_orient_matrix_UB_23      0.0234106000
_diffrn_orient_matrix_UB_31      0.0099730000
_diffrn_orient_matrix_UB_32      0.0430770000
_diffrn_orient_matrix_UB_33      -0.0029746000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            283178
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.819
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       plate
_exptl_crystal_F_000             2202
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.263
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1164
_refine_ls_number_reflns         25066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0444P)^2^+0.9100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20549
_reflns_number_total             25066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02274f2.cif
_cod_data_source_block           tlgxr121
_cod_depositor_comments
'Adding full bibliography for 7719506--7719510.cif.'
_cod_database_code               7719509
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C118O4P8Rh4
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.887
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_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 Ternary CH refined with riding coordinates:
 C87(H87), C33(H33), C88(H88), C6(H6), C34(H34), C61(H61), C7(H7), C57(H57),
 C60(H60), C84(H84), C30(H30), C3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C104(H104), C44(H44), C98(H98), C94(H94), C25(H25), C106(H106),
 C20(H20), C23(H23), C83(H83), C52(H52), C95(H95), C79(H79), C73(H73), C91(H91),
  C29(H29), C17(H17), C92(H92), C64(H64), C43(H43), C42(H42), C27(H27),
 C93(H93), C50(H50), C14(H14), C67(H67), C41(H41), C110(H110), C26(H26),
 C22(H22), C82(H82), C107(H107), C16(H16), C77(H77), C40(H40), C103(H103),
 C81(H81), C28(H28), C97(H97), C108(H108), C80(H80), C53(H53), C15(H15),
 C65(H65), C74(H74), C66(H66), C100(H100), C71(H71), C10(H10), C68(H68),
 C102(H102), C56(H56), C21(H21), C13(H13), C46(H46), C96(H96), C109(H109),
 C76(H76), C54(H54), C48(H48), C75(H75), C37(H37), C49(H49), C101(H101),
 C55(H55), C11(H11), C47(H47), C12(H12), C69(H69), C39(H39), C70(H70), C38(H38),
  C113(H113), C112(H112)
2.c Idealised Me refined as rotating group:
 C111(H11A,H11B,H11C), C114(H11D,H11E,H11F)
;
_shelx_res_checksum              29191
_shelx_hkl_checksum              82837
_shelx_fab_checksum              21995
_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 1.147
_oxdiff_exptl_absorpt_empirical_full_min 0.913