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_7719510
_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         'C83 H66 N4 Na O3 P5 Rh2, 2(C2 H3 N)'
_chemical_formula_sum            'C87 H72 N6 Na O3 P5 Rh2'
_chemical_formula_weight         1633.16
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2018-03-02 deposited with the CCDC.	2025-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2977(4)
_cell_length_b                   18.7962(5)
_cell_length_c                   26.1377(8)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.493
_cell_measurement_theta_min      2.896
_cell_volume                     7515.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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_temperature      100.02
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'double mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            320262
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.698
_diffrn_reflns_theta_min         2.896
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.054
_exptl_absorpt_correction_T_max  0.5871
_exptl_absorpt_correction_T_min  0.4371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1140 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.7445.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.863
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         15390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_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^+16.2751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14304
_reflns_number_total             15390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02274f2.cif
_cod_data_source_block           cu_jb211_0m
_cod_depositor_comments
'Adding full bibliography for 7719506--7719510.cif.'
_cod_database_code               7719510
_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:
 C59(H59), C58(H58), C55(H55), C23(H23), C7(H7), C8(H8), C43(H43), C22(H22),
 C44(H44), C40(H40), C19(H19), C4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C62(H62), C65(H65), C11(H11), C33(H33), C14(H14), C30(H30), C15(H15),
 C29(H29), C54(H54), C12(H12), C18(H18), C27(H27), C50(H50), C51(H51), C66(H66),
  C32(H32), C69(H69), C39(H39), C16(H16), C35(H35), C64(H64), C26(H26),
 C13(H13), C68(H68), C17(H17), C28(H28), C47(H47), C67(H67), C63(H63), C31(H31),
  C53(H53), C52(H52), C38(H38), C49(H49), C71(H71), C36(H36), C48(H48),
 C73(H73), C37(H37), C72(H72), C75(H75), C74(H74)
2.c Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C83(H83A,H83B,H83C), C81(H81A,H81B,
 H81C), C85(H85A,H85B,H85C), C87(H87A,H87B,H87C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'