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_7719506
_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         'C92 H66 O2 P4 Rh2, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C104 H74 Cl4 O2 P4 Rh2'
_chemical_formula_weight         1827.13
_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     direct
_audit_creation_date             2017-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-02 deposited with the CCDC.	2025-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.944(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1660(15)
_cell_length_b                   19.595(2)
_cell_length_c                   17.999(3)
_cell_measurement_reflns_used    8501
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.8380
_cell_measurement_theta_min      2.3280
_cell_volume                     3852.9(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -350.17   8.83   1.00   10.00   9.83  -0.10 -30.17    --   359
  2  \f   -350.17   9.83   1.00   20.00  20.65  -0.10 -30.17    --   360
  3  \f     -9.83 350.17   1.00   20.00  87.21  -0.10  30.17    --   360
  4  \f   -340.18  19.82   1.00   20.00  22.40  -0.10 -58.55    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0120156000
_diffrn_orient_matrix_UB_12      0.0005451000
_diffrn_orient_matrix_UB_13      -0.0402653000
_diffrn_orient_matrix_UB_21      0.0590504000
_diffrn_orient_matrix_UB_22      0.0138612000
_diffrn_orient_matrix_UB_23      0.0013160000
_diffrn_orient_matrix_UB_31      0.0242679000
_diffrn_orient_matrix_UB_32      -0.0334132000
_diffrn_orient_matrix_UB_33      -0.0006877000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29787
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.521
_diffrn_reflns_theta_min         1.980
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.575
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.282
_refine_diff_density_min         -1.786
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0797
_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^)+(0.1521P)^2^+4.6946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6938
_reflns_number_total             9428
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9917\% 
 around [-0.00 1.00 0.00] (reciprocal) or [-0.01 1.00 0.01] (direct)
Component 3 rotated by 0.5475\% 
 around [0.23 0.07 -0.97] (reciprocal) or [0.30 0.05 -0.95] (direct)
;
_cod_data_source_file            d5dt02274f2.cif
_cod_data_source_block           mo_jb142_3_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7719506--7719510.cif.'
_cod_original_cell_volume        3853.0(10)
_cod_database_code               7719506
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C50H50Rh1P2Cl2O1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C31(H31), C19(H19), C4(H4), C1(H1), C34(H34), C20(H20), C16(H16),
 C35(H35)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C42(H42), C13(H13), C12(H12), C11(H11), C30(H30), C45(H45), C9(H9),
 C14(H14), C44(H44), C23(H23), C43(H43), C10(H10), C27(H27), C24(H24), C40(H40),
  C39(H39), C29(H29), C28(H28), C25(H25), C26(H26), C15(H15), C41(H41),
 C38(H38), C49(H49), C52(H52), C50(H50), C51(H51)
;
_shelx_res_checksum              9058
_shelx_hkl_checksum              49485
_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 2.088
_oxdiff_exptl_absorpt_empirical_full_min 0.489
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3