An aniline-bridged <i>bis</i>(pyrazolyl)alkane ligand for dizinc-catalysed ring-opening polymerization.
Naik, Pratyush K.; Gu, Zipeng; Comito, Robert J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17443–17447; doi:10.1039/d4dt02837f

data_7717214
_publ_section_title
;
 An aniline-bridged <i>bis</i>(pyrazolyl)alkane ligand for
 dizinc-catalysed ring-opening polymerization.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17443
_journal_page_last               17447
_journal_paper_doi               10.1039/d4dt02837f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H44 N9 Zn2, C32 H12 B F24'
_chemical_formula_sum            'C65 H58 B Cl2 F24 N9 Zn2'
_chemical_formula_weight         1633.65
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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   mixed
_audit_creation_date             2024-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-08-27 deposited with the CCDC.	2024-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                77.1250(10)
_cell_angle_beta                 76.3660(10)
_cell_angle_gamma                85.9300(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2518(3)
_cell_length_b                   13.6360(3)
_cell_length_c                   21.3029(4)
_cell_measurement_reflns_used    9302
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      65.75
_cell_measurement_theta_min      3.33
_cell_volume                     3646.25(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_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, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'narrow frame omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59186
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        66.032
_diffrn_reflns_theta_max         66.032
_diffrn_reflns_theta_min         3.325
_exptl_absorpt_coefficient_mu    2.440
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.5901
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       plate
_exptl_crystal_F_000             1652
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/Hexane'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         12262
_refine_ls_number_restraints     598
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0485P)^2^+3.3060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11530
_reflns_number_total             12262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02837f2.cif
_cod_data_source_block           PN2-022__XW399_sq
_cod_depositor_comments          'Adding full bibliography for 7717214.cif.'
_cod_database_code               7717214
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.654
_olex2_refinement_description
;
1. Restrained distances
 C7-F1C \\sim C7-F2C \\sim C7-F3C \\sim C7-F4C \\sim C7-F5C \\sim C7-F6C
 with sigma of 0.02
 F1C-F2C \\sim F2C-F3C \\sim F3C-F1C \\sim F4C-F5C \\sim F5C-F6C \\sim F6C-F4C
 with sigma of 0.04
 C57-F1C \\sim C57-F2C \\sim C57-F3C \\sim C57-F4C \\sim C57-F5C \\sim C57-F6C
 with sigma of 0.1
 C52A-F1A \\sim C52A-F2A \\sim C52A-F3A \\sim C52B-F4A \\sim C52B-F5A \\sim
C52B-F6A
 with sigma of 0.02
 F1A-F2A \\sim F2A-F3A \\sim F3A-F1A \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.04
 C42-F1A \\sim C42-F2A \\sim C42-F3A \\sim C42-F4A \\sim C42-F5A \\sim C42-F6A
 with sigma of 0.1
 C42-C52A \\sim C42-C52B
 with sigma of 0.02
 C65-F1B \\sim C65-F2B \\sim C65-F3B \\sim C65-F4B \\sim C65-F5B \\sim C65-F6B
 with sigma of 0.02
 F1B-F2B \\sim F2B-F3B \\sim F3B-F1B \\sim F4B-F5B \\sim F5B-F6B \\sim F6B-F4B
 with sigma of 0.04
 C48-F1B \\sim C48-F2B \\sim C48-F3B \\sim C48-F4B \\sim C48-F5B \\sim C48-F6B
 with sigma of 0.1
2. Uiso/Uaniso restraints and constraints
C57 \\sim C7 \\sim F1C \\sim F2C \\sim F3C \\sim F4C \\sim F5C \\sim F6C:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C42 \\sim C52A \\sim C52B \\sim F1A \\sim F2A \\sim F3A \\sim C52B \\sim F4A
\\sim F5A \\sim F6A: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C48 \\sim C65 \\sim F1B \\sim F2B \\sim F3B \\sim F4B \\sim F5B \\sim F6B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F1A) = Uanis(F6A)
Uanis(F2A) = Uanis(F4A)
Uanis(F3A) = Uanis(F5A)
Uanis(F2B) = Uanis(F4B)
Uanis(F3B) = Uanis(F5B)
Uanis(F1C) = Uanis(F6C)
Uanis(F2C) = Uanis(F4C)
Uanis(C52A) = Uanis(C52B)
3. Rigid body (RIGU) restrains
 C57, C7, F1C, F2C, F3C, F4C, F5C, F6C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C52A, C52B, F1A, F2A, F3A, C52B, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48, C65, F1B, F2B, F3B, F4B, F5B, F6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C52B)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(C52A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=FVAR(2)
 Sof(F4C)=Sof(F5C)=Sof(F6C)=1-FVAR(3)
 Sof(F1C)=Sof(F2C)=Sof(F3C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C28(H28A,H28B)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C16(H16), C24(H24), C25(H25), C26(H26), C31(H31), C41(H41),
 C43(H43), C45(H45), C47(H47), C49(H49), C51(H51), C54(H54), C56(H56), C58(H58),
  C60(H60), C62(H62), C64(H64)
5.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C29(H29A,H29B,
 H29C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              65094
_shelx_fab_checksum              34710
_olex2_submission_special_instructions 'No special instructions were received'