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_7061154
_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         'C43 H58 Cl2 N3 O3 Y, C4 H8 O'
_chemical_formula_sum            'C47 H66 Cl2 N3 O4 Y'
_chemical_formula_weight         896.83
_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                93.03(3)
_cell_angle_beta                 95.98(3)
_cell_angle_gamma                110.98(3)
_cell_formula_units_Z            2
_cell_length_a                   11.362(2)
_cell_length_b                   13.161(3)
_cell_length_c                   17.005(3)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.89
_cell_volume                     2350.2(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker D8 Venture diffractrometer'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.968
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            90047
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.582
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1330 before and 0.0903 after correction.
The Ratio of minimum to maximum transmission is 0.7590.
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    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10520
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0515P)^2^+3.2798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8742
_reflns_number_total             10520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05548h2.cif
_cod_data_source_block           complex3
_cod_depositor_comments
'Adding full bibliography for 7061153--7061161.cif.'
_cod_original_cell_volume        2350.2(9)
_cod_database_code               7061154
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.748
_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
 O1A-C1A = O1A-C4A
 1.43 with sigma of 0.01
 C4A-C3A = C3A-C2A = C2A-C1A
 1.54 with sigma of 0.01
 O3-C43A = O3-C43 = O3-C40 = O3-C40A
 1.43 with sigma of 0.01
 C41-C40 = C41A-C40A = C42A-C41A = C42-C41 = C43-C42 = C43A-C42A
 1.54 with sigma of 0.01
 C2B-C1B = C3B-C2B = C4B-C3B
 1.54 with sigma of 0.01
 O1B-C4B = O1B-C1B
 1.43 with sigma of 0.01
 C43A-C41A = C42A-C40A = C40-C42 = C43-C41
 2.515 with sigma of 0.02
 C4A-C2A = C1A-C3A
 2.515 with sigma of 0.02
 C40-C43 = C43A-C40A
 2.336 with sigma of 0.02
 C1A-C4A
 2.336 with sigma of 0.02
 C4B-C2B = C3B-C1B
 2.515 with sigma of 0.02
 C1B-C4B
 2.336 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C2B \\sim C1B \\sim O1B \\sim
C3B \\sim C4B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Rigid body (RIGU) restrains
 C42, C41, C40, C43, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C43A, C42A, C41A, O3, C40A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1A, O1A, C4A, C2A, C3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C2B, C3B, O1B, C4B, C1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=
 Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=1-FVAR(1)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(1)
 Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(O1B)=Sof(C3B)=
 Sof(H3BA)=Sof(H3BB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=1-FVAR(2)
 Sof(O1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29)
6.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C40A(H40C,H40D), C41(H41A,H41B), C41A(H41C,H41D), C42(H42A,H42B), C42A(H42C,
 H42D), C43(H43A,H43B), C43A(H43C,H43D), C1A(H1AA,H1AB), C2A(H2AA,H2AB),
 C3A(H3AA,H3AB), C4A(H4AA,H4AB), C2B(H2BA,H2BB), C1B(H1BA,H1BB), C3B(H3BA,H3BB),
  C4B(H4BA,H4BB)
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)
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)
;
_shelx_res_checksum              58214
_olex2_submission_special_instructions 'No special instructions were received'