A binuclear guanidinate yttrium carbyne complex: unique reactivity toward unsaturated C-N, C-O and C-S bonds.
Jiang, Wen; Kong, Feng; Del Rosal, Iker; Li, Meng; Wang, Kai; Maron, Laurent; Zhang, Lixin; Chemical science 14 (2023) 9154–9160; doi:10.1039/d3sc03483f

data_1569612
_publ_section_title
;
 A binuclear guanidinate yttrium carbyne complex: unique reactivity toward
 unsaturated C-N, C-O and C-S bonds.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              9154
_journal_page_last               9160
_journal_paper_doi               10.1039/d3sc03483f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C47 H72 Al2 N3 Y'
_chemical_formula_sum            'C47 H72 Al2 N3 Y'
_chemical_formula_weight         821.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0717(3)
_cell_length_b                   12.1069(3)
_cell_length_c                   36.4308(9)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      53.82
_cell_measurement_theta_min      3.346
_cell_volume                     4883.3(2)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            29693
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        52.985
_diffrn_reflns_theta_max         52.985
_diffrn_reflns_theta_min         3.630
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_T_max  0.8636
_exptl_absorpt_correction_T_min  0.5888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1397 before and 0.0689 after correction. The Ratio of minimum to maximum transmission is 0.6818. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.079
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.00059(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8569
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+2.5311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                7743
_reflns_number_total             8569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03483f2.cif
_cod_data_source_block           ga_80522c_a
_cod_depositor_comments
'Adding full bibliography for 1569608--1569615.cif.'
_cod_database_code               1569612
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.796
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(2)
 0.03(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H,H,H,H,H,H,H,H,H,H,H) groups
3. Restrained distances
 C5-H5B = C5-H5A = C5-H5C = C6-H6B = C6-H6A = C6-H6C
 0.98 with sigma of 0.02
 H6B-H6C
 1.6 with sigma of 0.02
 H6A-H6C
 1.6 with sigma of 0.02
 H6A-H6B
 1.6 with sigma of 0.02
 H5A-H5C
 1.6 with sigma of 0.02
 H5C-H5B
 1.6 with sigma of 0.02
 H5B-H5A
 1.6 with sigma of 0.02
 C6-H6C
 0.98 with sigma of 0.02
 C1-H1C = C1-H1B = C1-H1A = C2-H2C = C2-H2B = C2-H2A
 0.98 with sigma of 0.02
 H6C-H6A \\sim H6A-H6B
 with sigma of 0.02
 H6A-H6B \\sim H6B-H6C
 with sigma of 0.02
 H6B-H6C \\sim H6C-H6A
 with sigma of 0.02
 H5A-H5B \\sim H5B-H5C
 with sigma of 0.02
 H5B-H5C \\sim H5C-H5A
 with sigma of 0.02
 H5C-H5A \\sim H5A-H5B
 with sigma of 0.02
 H6A-C5 \\sim C5-H6B
 with sigma of 0.02
 H6A-C5 \\sim C5-H6C
 with sigma of 0.02
 H6B-C5 \\sim C5-H6C
 with sigma of 0.02
 H5B-C6 \\sim C6-H5C
 with sigma of 0.02
 H5B-C6 \\sim C6-H5A
 with sigma of 0.02
 H5A-C6 \\sim C6-H5C
 with sigma of 0.02
4.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
4.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C41(H41A,H41B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C24(H24), C25(H25), C26(H26), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47)
4.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C)
;
_olex2_submission_special_instructions 'No special instructions were received'