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_7701100
_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, C63 H41 B2 F30 N2 Na O6'
_chemical_formula_sum            'C64 H43 B2 Cl2 F30 N2 Na O6'
_chemical_formula_weight         1621.51
_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   geom
_audit_creation_date             2019-05-30
_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                90.069(3)
_cell_angle_beta                 104.596(3)
_cell_angle_gamma                106.610(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2126(18)
_cell_length_b                   16.759(2)
_cell_length_c                   17.209(3)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      2.44
_cell_volume                     3256.1(8)
_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      100.01
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58618
_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         27.995
_diffrn_reflns_theta_min         1.227
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0463 before and 0.0408 after correction. The Ratio of minimum to maximum transmission is 0.9516. 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    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.396
_exptl_crystal_size_min          0.378
_refine_diff_density_max         2.933
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.117
_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     1011
_refine_ls_number_reflns         15632
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0943
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1568P)^2^+9.3957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2663
_refine_ls_wR_factor_ref         0.2963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10815
_reflns_number_total             15632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03511g3.cif
_cod_data_source_block           solve_mz_a
_cod_depositor_comments
'Adding full bibliography for 7701086--7701108.cif.'
_cod_original_cell_volume        3256.2(8)
_cod_database_code               7701100
_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 C(H,H,H) groups
2. Restrained distances
 Na1-O5
 2.3 with sigma of 0.01
 C51-O5
 1.45 with sigma of 0.01
 O5-C48
 1.45 with sigma of 0.01
 C51-C50
 1.57 with sigma of 0.01
 C48-C49
 1.57 with sigma of 0.01
 C50-C49
 1.53 with sigma of 0.01
 O4-C55
 1.47 with sigma of 0.02
 O4-C52
 1.47 with sigma of 0.02
 C55-C54
 1.53 with sigma of 0.02
 C54-C53
 1.53 with sigma of 0.02
 C53-C52
 1.53 with sigma of 0.02
 C56-C57
 1.53 with sigma of 0.02
 C58-C57
 1.53 with sigma of 0.02
 C58-C59
 1.53 with sigma of 0.02
 O3-C59
 1.47 with sigma of 0.02
 C56-O3
 1.47 with sigma of 0.02
 O5-C50
 2.39 with sigma of 0.01
 O5-C49
 2.39 with sigma of 0.01
 C51-C49
 2.39 with sigma of 0.01
 C50-C48
 2.39 with sigma of 0.01
 C51-Na1
 3.3 with sigma of 0.01
 C48-Na1
 3.3 with sigma of 0.01
 O3-C57
 2.36 with sigma of 0.04
 C56-C59
 2.36 with sigma of 0.04
 C56-C58
 2.36 with sigma of 0.04
 C59-C57
 2.36 with sigma of 0.04
 O4-C54
 2.36 with sigma of 0.04
 C52-C55
 2.36 with sigma of 0.04
 C53-C55
 2.36 with sigma of 0.04
 C54-O4
 2.36 with sigma of 0.04
3. Rigid bond restraints
 C51, C50, C49, C48, O5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 O5A, C48A, C49A, C50A, C51A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O5 \\sim C51 \\sim C50 \\sim C49 \\sim C48: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.08
C51A \\sim C50A \\sim C49A \\sim C48A \\sim O5A: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.08
Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.2
Uanis(O3) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.2
5. Others
 Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(O5A)=Sof(C50A)=Sof(H50C)=Sof(H50D)=
 Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(O5)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=
 Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C52(H52A,H52B), C53(H53A,H53B), C60(H60A,H60B), C62(H62A,
 H62B), C63(H63A,H63B), C61(H61A,H61B), C58(H58A,H58B), C51(H51A,H51B),
 C54(H54A,H54B), C56(H56A,H56B), C59(H59A,H59B), C57(H57A,H57B), C48(H48A,H48B),
  C49(H49A,H49B), C50(H50A,H50B), C55(H55A,H55B), C51A(H51C,H51D), C50A(H50C,
 H50D), C49A(H49C,H49D), C48A(H48C,H48D)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C1(H1), C6(H6), C2(H2), C9(H9), C8(H8)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              18492
_olex2_submission_special_instructions 'No special instructions were received'