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_7701092
_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         'C20 H40 Na O5, C47 H5 B2 F36 N2'
_chemical_formula_sum            'C67 H45 B2 F36 N2 Na O5'
_chemical_formula_weight         1686.66
_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             2019-05-24
_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                 106.941(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.937(3)
_cell_length_b                   25.254(4)
_cell_length_c                   18.608(3)
_cell_measurement_reflns_used    9082
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.57
_cell_volume                     7164(2)
_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      100.01
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62821
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.897
_diffrn_reflns_theta_min         1.400
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0489 before and 0.0430 after correction. The Ratio of minimum to maximum transmission is 0.8628. 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    1.564
_exptl_crystal_description       prism
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         16890
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0558P)^2^+16.6377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9872
_reflns_number_total             16890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03511g3.cif
_cod_data_source_block           mo_6004_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7701086--7701108.cif.'
_cod_database_code               7701092
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.930
_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
2. Restrained distances
 O5-C48A
 1.43 with sigma of 0.02
 C48A-C49
 1.53 with sigma of 0.02
 C48-C49
 1.53 with sigma of 0.02
 C48-O5
 1.43 with sigma of 0.02
 C60A-O1
 1.43 with sigma of 0.02
 C60-O1
 1.43 with sigma of 0.02
 C60A-C61
 1.53 with sigma of 0.02
 C60-C61
 1.53 with sigma of 0.02
 C48-C50
 2.37 with sigma of 0.04
 C48A-C50
 2.37 with sigma of 0.04
 C49-C51
 2.37 with sigma of 0.04
 C48-C51
 2.37 with sigma of 0.04
 C60A-C63
 2.37 with sigma of 0.04
 C60A-C62
 2.37 with sigma of 0.04
 C61-C63
 2.37 with sigma of 0.04
 C60-C63
 2.37 with sigma of 0.04
 C48A-C51
 2.37 with sigma of 0.001
3. Rigid bond restraints
 C60A, C61, O1, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, C48, C48A, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1A, F3A, F2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C49 \\sim C48 \\sim O5 \\sim C48A: within 1.7A with sigma of 0.05 and sigma for
terminal atoms of 0.08
O1 \\sim C60A \\sim C60 \\sim C61: within 1.7A with sigma of 0.05 and sigma for
terminal atoms of 0.08
F3A \\sim F1A \\sim F2A: within 1.7A with sigma of 0.05 and sigma for terminal
atoms of 0.08
5. Others
 Sof(H49C)=Sof(H49D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(H49A)=Sof(H49B)=Sof(C48)=Sof(H48A)=Sof(H48B)=FVAR(1)
 Sof(H61C)=Sof(H61D)=Sof(C60A)=Sof(H60C)=Sof(H60D)=1-FVAR(2)
 Sof(H61A)=Sof(H61B)=Sof(C60)=Sof(H60A)=Sof(H60B)=FVAR(2)
 Sof(F3A)=Sof(F1A)=Sof(F2A)=1-FVAR(3)
 Sof(F3)=Sof(F1)=Sof(F2)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C49(H49A,H49B), C49(H49C,H49D), C58(H58A,H58B), C51(H51A,
 H51B), C66(H66A,H66B), C55(H55A,H55B), C67(H67A,H67B), C59(H59A,H59B),
 C61(H61A,H61B), C61(H61C,H61D), C65(H65A,H65B), C63(H63A,H63B), C62(H62A,H62B),
  C64(H64A,H64B), C56(H56A,H56B), C60(H60A,H60B), C48(H48A,H48B), C54(H54A,
 H54B), C57(H57A,H57B), C52(H52A,H52B), C53(H53A,H53B), C48A(H48C,H48D),
 C60A(H60C,H60D)
6.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C39(H39), C41(H41), C45(H45), C43(H43)
;
_shelx_res_checksum              52724
_shelx_fab_checksum              41098
_olex2_submission_special_instructions 'No special instructions were received'