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_7061158
_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 Yb, C4 H8 O1'
_chemical_formula_sum            'C47 H66 Cl2 N3 O4 Yb'
_chemical_formula_weight         980.96
_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                93.34(9)
_cell_angle_beta                 95.90(4)
_cell_angle_gamma                111.100(10)
_cell_formula_units_Z            2
_cell_length_a                   11.400(10)
_cell_length_b                   13.189(12)
_cell_length_c                   17.09(5)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      27.392
_cell_measurement_theta_min      2.325
_cell_volume                     2372(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART APEX II 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      298.15
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX II 298K'
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27740
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         1.204
_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    2.127
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1378 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.2762.
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    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.625
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         10701
_refine_ls_number_restraints     566
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0454P)^2^+0.1057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9101
_reflns_number_total             10701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05548h2.cif
_cod_data_source_block           complex5
_cod_depositor_comments
'Adding full bibliography for 7061153--7061161.cif.'
_cod_database_code               7061158
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.652
_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
 C35-C34 = C34-C33 = C42-C41 = C43-C42
 1.54 with sigma of 0.01
 C1A-O1A = O1A-C4A
 1.43 with sigma of 0.01
 C2A-C1A = C3A-C2A = C4A-C3A
 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
 C35-C34 = C35A-C34A = C34A-C33A = C34-C33 = C33A-C32A = C33-C32
 1.54 with sigma of 0.01
 C37-C36 = C37A-C36A = C39A-C38A = C39-C38 = C38-C37 = C38A-C37A
 1.54 with sigma of 0.01
 O1-C32 = O1-C32A = O1-C35 = O1-C35A
 1.43 with sigma of 0.01
 O2-C36 = O2-C36A = O2-C39 = O2-C39A
 1.43 with sigma of 0.01
 C1A-C4A
 2.336 with sigma of 0.02
 C4A-C2A = C3A-C1A
 2.515 with sigma of 0.02
 C3B-C1B = C2B-C4B
 2.515 with sigma of 0.02
 C4B-C1B
 2.336 with sigma of 0.02
 C35-C32 = C35A-C32A
 2.336 with sigma of 0.02
 C39A-C36A = C39-C36
 2.336 with sigma of 0.02
 C39A-C37A \\sim C36A-C38A \\sim C39-C37 \\sim C36-C38
 with sigma of 0.02
 C32-C34 \\sim C35-C33 \\sim C32A-C34A \\sim C35A-C33A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1B \\sim C3B \\sim C2B \\sim C4B \\sim C1B \\sim O1A \\sim C1A \\sim C4A \\sim
C2A \\sim C3A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C32 \\sim C33 \\sim C34 \\sim C35 \\sim C32A \\sim C33A \\sim C34A \\sim C35A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C37A \\sim C38A \\sim C39A \\sim C36A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C4B, C3B, C2B, C1B, O1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C3A, O1A, C1A, C4A, C2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C35, C34, C33, O1, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C35A, C34A, C33A, O1, C32A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C38A, C39A, O2, C37A, C36A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C38, C39, O2, C37, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(O1B)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=1-FVAR(1)
 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(1)
 Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C34A)=
 Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=1-FVAR(2)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=FVAR(2)
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=
 Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=1-FVAR(3)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=
 Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(3)
 Fixed X: C2B(0.155901)
 Fixed Y: C2B(0.80989)
 Fixed Z: C2B(0.61007)
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),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C1A(H1AA,H1AB), C2A(H2AA,H2AB),
  C3A(H3AA,H3AB), C4A(H4AA,H4AB), C3B(H3BA,H3BB), C2B(H2BA,H2BB), C1B(H1BA,
 H1BB), C4B(H4BA,H4BB), C32A(H32C,H32D), C33A(H33C,H33D), C34A(H34C,H34D),
 C35A(H35C,H35D), C36A(H36C,H36D), C37A(H37C,H37D), C38A(H38C,H38D), C39A(H39C,
 H39D)
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              23674
_olex2_submission_special_instructions 'No special instructions were received'