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_7061153
_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 H50 N3 Na O2'
_chemical_formula_sum            'C39 H50 N3 Na O2'
_chemical_formula_weight         615.81
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 106.488(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6032(13)
_cell_length_b                   15.0919(15)
_cell_length_c                   20.395(2)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      3.10
_cell_volume                     3719.7(7)
_computing_data_collection       'Bruker SMART APEX II diffractrometer'
_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      300.00
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1157
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            144408
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.101
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1147 before and 0.0666 after correction.
The Ratio of minimum to maximum transmission is 0.7183.
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    1.100
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0047(9)
_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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6530
_refine_ls_number_restraints     322
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0721P)^2^+2.7370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.2017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3888
_reflns_number_total             6530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05548h2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
'Adding full bibliography for 7061153--7061161.cif.'
_cod_original_cell_volume        3719.8(7)
_cod_database_code               7061153
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.983
_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
 C38A-C37A = C39A-C38A = C37A-C36A
 1.54 with sigma of 0.01
 C38A-C36A \\sim C39A-C37A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C39A \\sim C39 \\sim C38 \\sim C38A \\sim C37A \\sim C36A \\sim C36 \\sim C37
\\sim C34 \\sim C34A \\sim C33A \\sim C33 \\sim C32A \\sim C35 \\sim C35A \\sim
C32: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C36A, C37A, C38A, O2, C39A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C33, C34, C35, C32, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C35A, C34A, C33A, O1, C32A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C38, C37, C36, C39, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C37A)=
 Sof(H37C)=Sof(H37D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(1)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C37)=Sof(H37A)=
 Sof(H37B)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(1)
 Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=1-FVAR(2)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(C33)=Sof(H33A)=Sof(H33B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C2(H2), C3(H3)
6.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B), C37(H37A,
 H37B), C39(H39A,H39B), C34(H34A,H34B), C33(H33A,H33B), C39A(H39C,H39D),
 C38A(H38C,H38D), C37A(H37C,H37D), C36A(H36C,H36D), C32A(H32C,H32D), C33A(H33C,
 H33D), C35A(H35C,H35D), C34A(H34C,H34D)
6.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C19(H19), C18(H18), C17(H17), C16(H16),
 C15(H15), C11(H11), C10(H10), C9(H9), C8(H8)
6.d Fitted pentagon refined as free rotating group:
 C4(N1,C1,C2,C3)
6.e Fitted hexagon refined as free rotating group:
 C20(C21,C22,C23,C24,C25), C14(C19,C18,C17,C16,C15)
6.f Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C27(H27A,H27B,
 H27C), C6(H6A,H6B,H6C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              97933
_olex2_submission_special_instructions 'No special instructions were received'