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_7719508
_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         'C49 H38 N O P2 Rh'
_chemical_formula_sum            'C49 H38 N O P2 Rh'
_chemical_formula_weight         821.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-01-10 deposited with the CCDC.	2025-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 105.834(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   9.541(5)
_cell_length_b                   17.905(5)
_cell_length_c                   11.316(5)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.49
_cell_volume                     1859.8(14)
_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      100.0
_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 0.998
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35758
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.408
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0605 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.8858.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0201P)^2^+2.0553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3606
_reflns_number_total             3940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02274f2.cif
_cod_data_source_block           mo_tlgxr86
_cod_depositor_comments
'Adding full bibliography for 7719506--7719510.cif.'
_cod_database_code               7719508
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C23B) = Uanis(C23A)
3. Others
 Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C24)=Sof(H24)=Sof(C28)=Sof(H28)=
 Sof(C27)=Sof(H27)=1-FVAR(1)
 Sof(C30)=Sof(H30)=Sof(C29)=Sof(H29)=Sof(C31)=Sof(H31)=Sof(C33)=Sof(H33)=
 Sof(C32)=Sof(H32)=FVAR(1)
 Sof(C23B)=1-FVAR(2)
 Sof(C23A)=FVAR(2)
 Fixed Sof: O1(0.5) C1(0.5) C17(0.5) C22(0.5) H22(0.5) C21(0.5) H21(0.5)
 C20(0.5) H20(0.5) C19(0.5) H19(0.5) C18(0.5) H18(0.5)
4.a Ternary CH refined with riding coordinates:
 N1(H1), C2(H2), C6(H6), C5(H5)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C16(H16), C12(H12), C13(H13), C9(H9), C10(H10), C11(H11),
 C30(H30), C29(H29), C31(H31), C25(H25), C26(H26), C24(H24), C33(H33), C32(H32),
  C28(H28), C27(H27), C22(H22), C21(H21), C20(H20), C19(H19), C18(H18)
4.c Fitted hexagon refined as free rotating group:
 C17(C22,C21,C20,C19,C18)
;
_shelx_res_checksum              19679
_shelx_hkl_checksum              63787
_olex2_submission_special_instructions 'No special instructions were received'