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_7701088
_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         'C60 H37 B2 F30 N2 Na O4.5, 2(C4 H8 O)'
_chemical_formula_sum            'C68 H53 B2 F30 N2 Na O6.5'
_chemical_formula_weight         1616.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-05-28
_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                91.293(2)
_cell_angle_beta                 91.963(2)
_cell_angle_gamma                107.760(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7032(13)
_cell_length_b                   13.4507(13)
_cell_length_c                   20.407(2)
_cell_measurement_reflns_used    5406
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.51
_cell_volume                     3316.8(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.95
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.927
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32050
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.061
_diffrn_reflns_theta_min         0.999
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0409 before and 0.0355 after correction. The Ratio of minimum to maximum transmission is 0.9119. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.287
_refine_diff_density_max         0.823
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         14919
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1930
_refine_ls_R_factor_gt           0.1031
_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^)+(0.1925P)^2^+4.6573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2907
_refine_ls_wR_factor_ref         0.3639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7041
_reflns_number_total             14919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03511g3.cif
_cod_data_source_block           mo_5636_0m_a
_cod_depositor_comments
'Adding full bibliography for 7701086--7701108.cif.'
_cod_original_cell_volume        3316.7(6)
_cod_original_formula_sum        'C68 H53 B2 F30 N2 Na O6.50'
_cod_database_code               7701088
_shelx_shelxl_version_number     2018/3
_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 O(H) groups
2. Restrained distances
 O1-H1
 0.87 with sigma of 0.01
 C47-C48
 1.52 with sigma of 0.02
 C48-C49
 1.52 with sigma of 0.02
 O3-C50
 1.43 with sigma of 0.001
 O3-C47
 1.43 with sigma of 0.001
 C50-C49
 1.53 with sigma of 0.001
 C49-C48
 1.53 with sigma of 0.001
 C48-C47
 1.53 with sigma of 0.001
 C46-H1
 1.896644 with sigma of 0.02
 Na1-H1
 2.811397 with sigma of 0.02
 C48-C50
 2.38 with sigma of 0.04
 C47-C49
 2.38 with sigma of 0.04
 C50-C48
 2.37 with sigma of 0.001
 C49-C47
 2.37 with sigma of 0.001
 O3-C48
 2.37 with sigma of 0.001
 O3-C49
 2.37 with sigma of 0.001
3. Rigid bond restraints
 C47, C48, C49, C50, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C55, O2, C56, C57, C58
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 O4, C54, C53, C52, C51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C64, C66, C65, C63, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C47 \\sim C48 \\sim C49 \\sim C50 \\sim O3: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.08
C55 \\sim C56 \\sim C57 \\sim C58 \\sim O2: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.08
O3 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.08
C51 \\sim C52 \\sim C53 \\sim C54 \\sim O4: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.08
O6 \\sim C63 \\sim C65 \\sim C66 \\sim C64: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: O3(0.5) C50(0.5) H50A(0.5) H50B(0.5) C48(0.5) H48A(0.5) H48B(0.5)
 C49(0.5) H49A(0.5) H49B(0.5) C47(0.5) H47A(0.5) H47B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C59(H59A,H59B), C63(H63A,H63B), C64(H64A,H64B), C60(H60A,
 H60B), C66(H66A,H66B), C61(H61A,H61B), C62(H62A,H62B), C70(H70A,H70B),
 C58(H58A,H58B), C69(H69A,H69B), C67(H67A,H67B), C68(H68A,H68B), C52(H52A,H52B),
  C57(H57A,H57B), C56(H56A,H56B), C53(H53A,H53B), C51(H51A,H51B), C54(H54A,
 H54B), C65(H65A,H65B), C55(H55A,H55B), C50(H50A,H50B), C48(H48A,H48B),
 C49(H49A,H49B), C47(H47A,H47B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C45(H45), C41(H41), C44(H44), C42(H42)
;
_shelx_res_checksum              44246
_olex2_submission_special_instructions 'No special instructions were received'