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_7719507
_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         'C56 H42 O2 P4 Rh2, 2(C4 H8 O)'
_chemical_formula_sum            'C64 H58 O4 P4 Rh2'
_chemical_formula_weight         1220.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8929(5)
_cell_length_b                   28.2041(7)
_cell_length_c                   12.3931(3)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.01
_cell_measurement_theta_min      3.13
_cell_volume                     6254.2(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0567
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            97175
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        65.246
_diffrn_reflns_theta_max         65.246
_diffrn_reflns_theta_min         3.134
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.572
_exptl_absorpt_correction_T_max  0.5835
_exptl_absorpt_correction_T_min  0.4144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1109 before and 0.0797 after correction. The Ratio of minimum to maximum transmission is 0.7102. The \l/2 correction factor is Not present.'
_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    1.297
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.349
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0238P)^2^+33.4854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4810
_reflns_number_total             5429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02274f2.cif
_cod_data_source_block           jb205
_cod_depositor_comments
'Adding full bibliography for 7719506--7719510.cif.'
_cod_database_code               7719507
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.434
_shelx_estimated_absorpt_t_min   0.286
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Sof(H30C)=Sof(H30D)=Sof(H33C)=Sof(H33D)=Sof(C31)=Sof(H31A)=Sof(H31B)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(H33A)=Sof(H33B)=Sof(C32)=Sof(H32A)=Sof(H32B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C5(H5), C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30C,H30D), C30(H30A,H30B), C33(H33C,H33D), C33(H33A,
 H33B), C31(H31A,H31B), C32(H32A,H32B)
3.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C18(H18), C11(H11), C9(H9), C24(H24), C22(H22), C19(H19), C12(H12),
 C26(H26), C21(H21), C10(H10), C27(H27), C20(H20), C25(H25), C13(H13), C15(H15),
  C14(H14), C16(H16)
;
_shelx_res_checksum              31377
_shelx_hkl_checksum              34816
_shelx_fab_checksum              64998
_olex2_submission_special_instructions 'No special instructions were received'