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_7717611
_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         'C42 H59 Al Lu N2 P'
_chemical_formula_sum            'C42 H59 Al Lu N2 P'
_chemical_formula_weight         824.83
_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.cc2l67hk
_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                 92.4820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7487(5)
_cell_length_b                   18.7568(7)
_cell_length_c                   17.9516(7)
_cell_measurement_reflns_used    9757
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.529
_cell_measurement_theta_min      2.450
_cell_volume                     4288.6(3)
_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      192.83
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.0288
_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       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45965
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.206
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.388
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1314 before and 0.0604 after correction. The Ratio of minimum to maximum transmission is 0.8274. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0102P)^2^+3.3890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6497
_reflns_number_total             7578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03060e2.cif
_cod_data_source_block           mo_220602b_a
_cod_depositor_comments
'Adding full bibliography for 7717606--7717614.cif.'
_cod_database_code               7717611
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.587
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H18a,H18b,H18c} of C18
 At 1.5 times of:
  {H1a,H1b,H1c} of C1, {H4a,H4b,H4c} of C4, {H5a,H5b,H5c} of C5, {H26a,H26b,
  H26c} of C26, {H30a,H30b,H30c} of C30, {H17a,H17b,H17c} of C17, {H15a,H15b,
  H15c} of C15, {H29a,H29b,H29c} of C29, {H27a,H27b,H27c} of C27, {H14a,H14b,
  H14c} of C14
2.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C14(H14a,H14b,H14c),
 C15(H15a,H15b,H15c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C26(H26a,H26b,
 H26c), C27(H27a,H27b,H27c), C29(H29a,H29b,H29c), C30(H30a,H30b,H30c)
;
_olex2_submission_special_instructions 'No special instructions were received'