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_7061161
_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         'C39 H56 N3 Si2 Y, 0.5(C6 H14)'
_chemical_formula_sum            'C42 H63 N3 Si2 Y'
_chemical_formula_weight         755.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 91.546(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.872(2)
_cell_length_b                   17.623(2)
_cell_length_c                   36.834(6)
_cell_measurement_reflns_used    9050
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.099
_cell_measurement_theta_min      2.473
_cell_volume                     9001(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker D8 Venture diffractrometer'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1292
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            145200
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.221
_diffrn_reflns_theta_min         2.151
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.378
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1366 before and 0.0882 after correction.
The Ratio of minimum to maximum transmission is 0.6978.
The \l/2 correction factor is Not present.
;
_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    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.00064(14)
_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   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         10965
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.0992
_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^)+(0.0580P)^2^+91.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2444
_refine_ls_wR_factor_ref         0.2766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5856
_reflns_number_total             10965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05548h2.cif
_cod_data_source_block           complex6
_cod_depositor_comments
'Adding full bibliography for 7061153--7061161.cif.'
_cod_database_code               7061161
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.609
_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
 C31-C29 = C30-C29 = C26-C21
 1.54 with sigma of 0.01
 C1A-C1B = C1B-C1C = C1C-C1D = C1D-C1E = C1E-C1F
 1.52 with sigma of 0.02
 C1A-C1C = C1D-C1F
 2.53 with sigma of 0.04
 C1B-C1D = C1C-C1E
 2.54 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F
 with sigma of 0.02
 C1A-C1C \\sim C1C-C1E \\sim C1B-C1D \\sim C1D-C1F
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C1E)
\\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1F) \\sim Ueq: with sigma of 0.004 and
sigma for terminal atoms of 0.008
4. Others
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) H1BA(0.5)
 H1BB(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) C1E(0.5)
 H1EA(0.5) H1EB(0.5) C1F(0.5) H1FA(0.5) H1FB(0.5) H1FC(0.5)
5.a Riding coordinates:
 C1A(H1AA,H1AB,H1AC), C1F(H1FA,H1FB,H1FC)
5.b Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C26(H26), C29(H29)
5.c Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C36(H36A,H36B), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,
 H1DB), C1E(H1EA,H1EB)
5.d Me refined with riding coordinates:
 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)
5.e Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C9(H9), C8(H8), C16(H16), C15(H15), C19(H19), C18(H18),
 C17(H17), C22(H22), C24(H24), C23(H23)
5.f Fitted hexagon refined as free rotating group:
 C11(C10,C9,C8,C7,C12), C16(C15,C14,C19,C18,C17), C22(C21,C20,C25,C24,C23)
;
_shelx_res_checksum              89804
_olex2_submission_special_instructions 'No special instructions were received'