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_7701087
_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         'C62 H40 B2 F30 N3 Na O5, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C62.5 H41 B2 Cl F30 N3 Na O5'
_chemical_formula_weight         1564.04
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-02
_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                 93.240(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3526(11)
_cell_length_b                   30.789(2)
_cell_length_c                   16.1477(13)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.35
_cell_volume                     6627.9(9)
_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)'
_diffrn_ambient_temperature      100.08
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0299
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64223
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.957
_diffrn_reflns_theta_min         1.426
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0445 before and 0.0389 after correction. The Ratio of minimum to maximum transmission is 0.9379. 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    1.567
_exptl_crystal_description       prism
_exptl_crystal_F_000             3140
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         15883
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0815
_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^)+(0.0857P)^2^+19.8698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12493
_reflns_number_total             15883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03511g3.cif
_cod_data_source_block           mo_5922_0m_a
_cod_depositor_comments
'Adding full bibliography for 7701086--7701108.cif.'
_cod_original_cell_volume        6627.8(9)
_cod_original_formula_sum        'C62.50 H41 B2 Cl F30 N3 Na O5'
_cod_database_code               7701087
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.927
_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
 O3-C52
 1.22 with sigma of 0.02
 C52-C53
 1.49 with sigma of 0.02
 C52-C54
 1.49 with sigma of 0.02
 C53-C54
 2.55 with sigma of 0.04
3. Rigid bond restraints
 C54, C52, C53, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, C63, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3 \\sim C52 \\sim C53 \\sim C54: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Cl2 \\sim C63 \\sim Cl1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) C63(0.5) H63A(0.5) H63B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C58(H58A,H58B), C57(H57A,H57B), C56(H56A,H56B), C62(H62A,
 H62B), C61(H61A,H61B), C60(H60A,H60B), C59(H59A,H59B), C63(H63A,H63B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C9(H9), C8(H8), C1(H1), C2(H2)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              5292
_olex2_submission_special_instructions 'No special instructions were received'