Phosphaguanidinate yttrium carbene, carbyne and carbide complexes: three distinct C1 functionalities.
Jiang, Wen; Zhang, Lixin; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2320–2330; doi:10.1039/d4dt03060e

data_7717612
_publ_section_title
;
 Phosphaguanidinate yttrium carbene, carbyne and carbide complexes: three
 distinct C1 functionalities.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2320
_journal_page_last               2330
_journal_paper_doi               10.1039/d4dt03060e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C64 H85 Lu N4 P'
_chemical_formula_sum            'C64 H85 Lu N4 P'
_chemical_formula_weight         1116.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2l67km
_audit_creation_date             2024-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-10-08 deposited with the CCDC.	2024-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.79(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.962(8)
_cell_length_b                   19.845(12)
_cell_length_c                   22.439(14)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      26.970
_cell_measurement_theta_min      2.240
_cell_volume                     5704(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      198.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59596
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         2.207
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.801
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1605 before and 0.0828 after correction. The Ratio of minimum to maximum transmission is 0.8547. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0257P)^2^+4.3789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7665
_reflns_number_total             10112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03060e2.cif
_cod_data_source_block           mo_220627a_1_a
_cod_depositor_comments
'Adding full bibliography for 7717606--7717614.cif.'
_cod_database_code               7717612
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.693
_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:
 C9(H9), C12(H12), C21(H21), C24(H24), C33(H33), C47(H47), C50(H50), C59(H59),
 C62(H62)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C43(H43), C44(H44), C45(H45), C55(H55), C56(H56), C57(H57)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C13(H13a,H13b,
 H13c), C14(H14a,H14b,H14c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C25(H25a,
 H25b,H25c), C26(H26a,H26b,H26c), C40(H40a,H40b,H40c), C48(H48a,H48b,H48c),
 C49(H49a,H49b,H49c), C51(H51a,H51b,H51c), C52(H52a,H52b,H52c), C60(H60a,H60b,
 H60c), C61(H61a,H61b,H61c), C63(H63a,H63b,H63c), C64(H64a,H64b,H64c)
;
_olex2_submission_special_instructions 'No special instructions were received'