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_7061160
_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 Er N3 Si2'
_chemical_formula_sum            'C39 H56 Er N3 Si2'
_chemical_formula_weight         790.30
_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                93.5150(10)
_cell_angle_beta                 98.1530(10)
_cell_angle_gamma                98.1800(10)
_cell_formula_units_Z            4
_cell_length_a                   11.4267(8)
_cell_length_b                   18.5276(13)
_cell_length_c                   20.0773(14)
_cell_measurement_reflns_used    9360
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      27.554
_cell_measurement_theta_min      2.224
_cell_volume                     4150.4(5)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker SMART APEX II 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      298.15
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0224
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47688
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.573
_diffrn_reflns_theta_min         1.028
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  0.6429
_exptl_absorpt_correction_T_min  0.6103
_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    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of n-hexane and toluene at RT.'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.913
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         18624
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+2.3364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15009
_reflns_number_total             18624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05548h2.cif
_cod_data_source_block           complex7
_cod_depositor_comments
'Adding full bibliography for 7061153--7061161.cif.'
_cod_database_code               7061160
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.643
_shelx_estimated_absorpt_t_min   0.610
_exptl_crystal_mounting_method
'The title complex was mounted in a sealed capillary.'
_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
 C74A-C72A \\sim C74A-C73A \\sim C73A-C72A
 with sigma of 0.02
 C74-C73 \\sim C73-C72 \\sim C74-C72
 with sigma of 0.02
 C35-C33 \\sim C35-C34 \\sim C34-C33
 with sigma of 0.02
 C34A-C33A \\sim C35A-C34A \\sim C35A-C33A
 with sigma of 0.02
 Si1-C34A \\sim Si1-C33 \\sim Si1-C33A \\sim Si1-C35 \\sim Si1-C35A \\sim
Si1-C34
 with sigma of 0.02
3. Rigid bond restraints
 C34, C35A, C35, C33A, C33, C34A, Si1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C35 \\sim C33 \\sim C34 \\sim C33A \\sim C35A \\sim C34A \\sim C73 \\sim C72
\\sim C74 \\sim C73A \\sim C72A \\sim C74A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(Si1) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C35A)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C33) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(C73A)=Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(C72A)=Sof(H72D)=Sof(H72E)=
 Sof(H72F)=Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(2)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C68(H68), C26(H26), C29(H29), C65(H65)
6.b Secondary CH2 refined with riding coordinates:
 C75(H75A,H75B), C71(H71A,H71B), C36(H36A,H36B), C32(H32A,H32B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C2(H2), C63(H63), C42(H42), C50(H50), C19(H19), C54(H54),
 C48(H48), C11(H11), C47(H47), C22(H22), C57(H57), C41(H41), C8(H8), C18(H18),
 C49(H49), C23(H23), C61(H61), C24(H24), C58(H58), C16(H16), C10(H10), C17(H17),
  C56(H56), C62(H62), C9(H9), C55(H55)
6.d Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C66(H66A,H66B,
 H66C), C78(H78A,H78B,H78C), C72(H72A,H72B,H72C), C44(H44A,H44B,H44C), C5(H5A,
 H5B,H5C), C76(H76A,H76B,H76C), C30(H30A,H30B,H30C), C6(H6A,H6B,H6C), C67(H67A,
 H67B,H67C), C70(H70A,H70B,H70C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C),
 C39(H39A,H39B,H39C), C74(H74A,H74B,H74C), C69(H69A,H69B,H69C), C77(H77A,H77B,
 H77C), C45(H45A,H45B,H45C), C37(H37A,H37B,H37C), C27(H27A,H27B,H27C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C33A(H33D,H33E,H33F), C35A(H35D,H35E,H35F),
 C34A(H34D,H34E,H34F), C73A(H73D,H73E,H73F), C72A(H72D,H72E,H72F), C74A(H74D,
 H74E,H74F)
;
_shelx_res_checksum              38601
_olex2_submission_special_instructions 'No special instructions were received'