Synthesis, structure, and coordination chemistry of a neutral pyrrolyl-functionalized amidinate ligand
Guo, Liping; Guo, Changjia; Peng, Shuqi; Song, Renyuan; New Journal of Chemistry 46 (2022) 2465–2471; doi:10.1039/D1NJ05548H

data_7061159
_publ_section_title
;
 Synthesis, structure, and coordination chemistry of a neutral
 pyrrolyl-functionalized amidinate ligand
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2465
_journal_page_last               2471
_journal_paper_doi               10.1039/D1NJ05548H
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         '1(C39 H56 N3 Si2 Yb)'
_chemical_formula_sum            'C39 H56 N3 Si2 Yb'
_chemical_formula_weight         796.08
_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   geom
_audit_creation_date             2021-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-15 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                93.4610(10)
_cell_angle_beta                 98.1800(10)
_cell_angle_gamma                97.8690(10)
_cell_formula_units_Z            4
_cell_length_a                   11.4008(10)
_cell_length_b                   18.4999(16)
_cell_length_c                   20.1152(18)
_cell_measurement_reflns_used    9740
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.27
_cell_volume                     4146.0(6)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker D8 Venture diffractrometer'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.00
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47293
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         1.026
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.341
_exptl_absorpt_correction_T_max  0.6392
_exptl_absorpt_correction_T_min  0.5922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.143
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         18538
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0274P)^2^+3.3092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15000
_reflns_number_total             18538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05548h2.cif
_cod_data_source_block           complex8
_cod_depositor_comments
'Adding full bibliography for 7061153--7061161.cif.'
_cod_database_code               7061159
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.592
_olex2_refinement_description
;
1. 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
2. Restrained distances
 Si2-C37 \\sim Si2-C38 \\sim Si2-C39 \\sim Si2-C37' \\sim Si2-C38' \\sim
Si2-C39'
 with sigma of 0.02
 Si4-C76 \\sim Si4-C77 \\sim Si4-C78 \\sim Si4-C76' \\sim Si4-C77' \\sim
Si4-C78'
 with sigma of 0.02
 C37-C38 \\sim C38-C39 \\sim C39-C37 \\sim C37'-C38' \\sim C38'-C39' \\sim
C39'-C37'
 with sigma of 0.02
 C76-C77 \\sim C77-C78 \\sim C78-C76 \\sim C76'-C77' \\sim C77'-C78' \\sim
C78'-C76'
 with sigma of 0.02
3. Rigid bond restraints
 Si2, C37, C38, C39, C37', C38', C39'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si4, C76, C77, C78, C76', C77', C78'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Si2 \\sim C37 \\sim C38 \\sim C39 \\sim C37' \\sim C38' \\sim C39': within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Si4 \\sim C76 \\sim C77 \\sim C78 \\sim C76' \\sim C77' \\sim C78': within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
5. Others
 Sof(C37')=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38')=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C39')=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C76')=Sof(H76D)=
 Sof(H76E)=Sof(H76F)=Sof(C77')=Sof(H77D)=Sof(H77E)=Sof(H77F)=Sof(C78')=
 Sof(H78D)=Sof(H78E)=Sof(H78F)=1-FVAR(1)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=
 FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C65(H65), C68(H68)
6.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C36(H36A,H36B), C71(H71A,H71B), C75(H75A,H75B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C41(H41), C42(H42),
  C47(H47), C48(H48), C49(H49), C50(H50), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58), C61(H61), C62(H62), C63(H63)
6.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C37'(H37D,H37E,H37F), C38'(H38D,H38E,H38F), C39'(H39D,H39E,H39F),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C),
 C78(H78A,H78B,H78C), C76'(H76D,H76E,H76F), C77'(H77D,H77E,H77F), C78'(H78D,
 H78E,H78F)
;
_shelx_res_checksum              83495
_olex2_submission_special_instructions 'No special instructions were received'