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_7717614
_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         'C84 H115 Al3 N4 P2 Y2'
_chemical_formula_sum            'C84 H115 Al3 N4 P2 Y2'
_chemical_formula_weight         1501.49
_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   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2l67nq
_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                 93.891(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8360(19)
_cell_length_b                   12.2333(12)
_cell_length_c                   34.501(3)
_cell_measurement_reflns_used    9731
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      59.334
_cell_measurement_theta_min      3.857
_cell_volume                     8352.7(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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      173.0
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            144943
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.999
_diffrn_reflns_theta_max         52.999
_diffrn_reflns_theta_min         3.823
_exptl_absorpt_coefficient_mu    1.886
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.4996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1651 before and 0.0987 after correction. The Ratio of minimum to maximum transmission is 0.6647. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.891
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         14774
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+12.9511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12668
_reflns_number_total             14774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03060e2.cif
_cod_data_source_block           ga_221113b_a
_cod_depositor_comments
'Adding full bibliography for 7717606--7717614.cif.'
_cod_database_code               7717614
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.728
_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
 H2c-H2a
 1.6 with sigma of 0.02
 H2c-H2b
 1.6 with sigma of 0.02
 C2-H2c
 1 with sigma of 0.01
 C2-H2b
 1 with sigma of 0.01
 C2-H2a
 1 with sigma of 0.01
 H2b-H2a
 1.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Y2) = Uanis(C2)
4.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C30(H30), C33(H33), C55(H55), C58(H58), C67(H67), C70(H70)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C26(H26), C27(H27), C28(H28), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C51(H51), C52(H52), C53(H53), C63(H63), C64(H64), C65(H65),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80), C81(H81), C82(H82),
  C83(H83), C84(H84)
4.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C7(H7a,H7b,H7c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c),
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C22(H22a,H22b,H22c), C23(H23a,H23b,
 H23c), C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C34(H34a,H34b,H34c), C35(H35a,
 H35b,H35c), C56(H56a,H56b,H56c), C57(H57a,H57b,H57c), C59(H59a,H59b,H59c),
 C60(H60a,H60b,H60c), C68(H68a,H68b,H68c), C69(H69a,H69b,H69c), C71(H71a,H71b,
 H71c), C72(H72a,H72b,H72c)
;
_olex2_submission_special_instructions 'No special instructions were received'