Imidazolyl-phenyl (IMP) anions: a modular structure for tuning solubility and coordinating ability.
Wozniak, Derek I.; Hicks, Andrew J.; Sabbers, William A.; Dobereiner, Graham E.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14138–14155; doi:10.1039/c9dt03511g

data_7701091
_publ_section_title
;
 Imidazolyl-phenyl (IMP) anions: a modular structure for tuning solubility
 and coordinating ability.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14138
_journal_page_last               14155
_journal_paper_doi               10.1039/c9dt03511g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C H2 Cl2, C62 H40 B2 F30 N3 Na O3'
_chemical_formula_sum            'C63 H42 B2 Cl2 F30 N3 Na O3'
_chemical_formula_weight         1574.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-30 deposited with the CCDC.    2019-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.217(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.184(3)
_cell_length_b                   15.7566(14)
_cell_length_c                   26.172(2)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      2.58
_cell_volume                     12922.0(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.04
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            118693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.931
_diffrn_reflns_theta_min         1.300
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0549 before and 0.0472 after correction. The Ratio of minimum to maximum transmission is 0.9091. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       prism
_exptl_crystal_F_000             6320
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.105
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1925
_refine_ls_number_reflns         30809
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.0933
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1259P)^2^+40.0219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2463
_refine_ls_wR_factor_ref         0.2826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18582
_reflns_number_total             30809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03511g3.cif
_cod_data_source_block           solve_a
_cod_depositor_comments
;
Adding full bibliography for 7701086--7701108.cif.

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        12922(2)
_cod_original_formula_moiety     '2(C H2 Cl2), 2(C62 H40 B2 F30 N3 Na O3)'
_cod_original_formula_sum        'C126 H84 B4 Cl4 F60 N6 Na2 O6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     3149.01
_cod_database_code               7701091
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid bond restraints
 C84, C83, C86, C85
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C76, C77, C78
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C45, C46, F1, C47, F2, C48, F3, C49, F4, C50, F5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C75 \\sim C76 \\sim C77 \\sim C78: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.08
C85 \\sim C86 \\sim O5 \\sim C83 \\sim C84: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.08
C45 \\sim C46 \\sim F1 \\sim C47 \\sim C48 \\sim F2 \\sim F3 \\sim F4 \\sim C49
\\sim C50 \\sim F5: within 1.7A with sigma of 0.01 and sigma for terminal atoms
of 0.08
4. Others
 Sof(H83C)=Sof(H83D)=Sof(H85C)=Sof(H85D)=Sof(C84A)=Sof(H84C)=Sof(H84D)=1-FVAR(1)
 Sof(H83A)=Sof(H83B)=Sof(H85A)=Sof(H85B)=Sof(C84)=Sof(H84A)=Sof(H84B)=FVAR(1)
 Sof(H75C)=Sof(H75D)=Sof(H78D)=Sof(H78E)=Sof(H78F)=Sof(C76A)=Sof(H76C)=
 Sof(H76D)=Sof(C77A)=Sof(H77C)=Sof(H77D)=1-FVAR(2)
 Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H78A)=Sof(H78B)=
 Sof(H78C)=Sof(C77)=Sof(H77A)=Sof(H77B)=FVAR(2)
 Sof(H11C)=Sof(H11D)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C12A)=Sof(H12C)=
 Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=1-FVAR(3)
 Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C13)=Sof(H13A)=Sof(H13B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C11(H11A,H11B), C11(H11C,
 H11D), C79(H79A,H79B), C75(H75A,H75B), C75(H75C,H75D), C81(H81A,H81B),
 C80(H80A,H80B), C25(H25A,H25B), C26(H26A,H26B), C64(H64A,H64B), C23(H23A,H23B),
  C19(H19A,H19B), C88(H88A,H88B), C87(H87A,H87B), C24(H24A,H24B), C90(H90A,
 H90B), C63(H63A,H63B), C22(H22A,H22B), C89(H89A,H89B), C12(H12A,H12B),
 C83(H83A,H83B), C83(H83C,H83D), C76(H76A,H76B), C13(H13A,H13B), C20(H20A,H20B),
  C21(H21A,H21B), C77(H77A,H77B), C86(H86A,H86B), C85(H85A,H85B), C85(H85C,
 H85D), C84(H84A,H84B), C84A(H84C,H84D), C76A(H76C,H76D), C77A(H77C,H77D),
 C12A(H12C,H12D), C13A(H13C,H13D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C66(H66), C65(H65), C73(H73), C9(H9), C72(H72), C5(H5),
 C6(H6), C8(H8), C69(H69), C70(H70)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C82(H82A,H82B,H82C), C14(H14A,H14B,H14C), C14(H14D,H14E,
 H14F), C78(H78A,H78B,H78C), C78(H78D,H78E,H78F)
;
_shelx_res_checksum              75481
_olex2_submission_special_instructions 'No special instructions were received'