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_7717613
_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         'C82 H110 Al2 N4 P2 Y2'
_chemical_formula_sum            'C82 H110 Al2 N4 P2 Y2'
_chemical_formula_weight         1445.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2l67ln
_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                66.611(2)
_cell_angle_beta                 78.717(2)
_cell_angle_gamma                79.637(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0176(6)
_cell_length_b                   18.7006(11)
_cell_length_c                   19.4040(11)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.386
_cell_measurement_theta_min      2.229
_cell_volume                     3899.7(4)
_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      193.29
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0978
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85131
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         2.216
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1667 before and 0.0785 after correction. The Ratio of minimum to maximum transmission is 0.6269. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         13652
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0288P)^2^+1.4177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10950
_reflns_number_total             13652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03060e2.cif
_cod_data_source_block           mo_220603c_a
_cod_depositor_comments
'Adding full bibliography for 7717606--7717614.cif.'
_cod_database_code               7717613
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.692
_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. Restrained distances
 C2-H2
 0.98 with sigma of 0.02
 C1-H1c
 0.98 with sigma of 0.02
 C1-H1a
 0.98 with sigma of 0.02
 H1c-H1b
 1.6 with sigma of 0.02
 H1b-H1a
 1.6 with sigma of 0.02
 H1c-H1a
 1.6 with sigma of 0.02
 C1-H1b
 0.96 with sigma of 0.02
3. Rigid bond restraints
 Y1, C1, Y2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.2 and sigma for terminal atoms of 0.4
5.a Ternary CH refined with riding coordinates:
 C28(H28), C68(H68), C16(H16), C31(H31), C65(H65), C19(H19), C56(H56), C53(H53)
5.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C61(H61), C35(H35), C82(H82), C72(H72), C24(H24), C41(H41),
 C78(H78), C43(H43), C45(H45), C79(H79), C14(H14), C25(H25), C36(H36), C12(H12),
  C63(H63), C39(H39), C80(H80), C76(H76), C62(H62), C44(H44), C74(H74),
 C81(H81), C51(H51), C75(H75), C49(H49), C73(H73), C42(H42), C13(H13), C37(H37),
  C38(H38), C50(H50)
5.c Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C70(H70a,H70b,H70c), C30(H30a,H30b,H30c), C69(H69a,H69b,
 H69c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C17(H17a,H17b,H17c), C18(H18a,
 H18b,H18c), C21(H21a,H21b,H21c), C29(H29a,H29b,H29c), C55(H55a,H55b,H55c),
 C66(H66a,H66b,H66c), C57(H57a,H57b,H57c), C20(H20a,H20b,H20c), C58(H58a,H58b,
 H58c), C4(H4a,H4b,H4c), C54(H54a,H54b,H54c), C67(H67a,H67b,H67c)
;
_olex2_submission_special_instructions 'No special instructions were received'