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_7701096
_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         'C82 H48 B2 F30 N6 O3 Pd, 5(C7 H8)'
_chemical_formula_sum            'C117 H88 B2 F30 N6 O3 Pd'
_chemical_formula_weight         2323.95
_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                 101.862(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6043(18)
_cell_length_b                   26.890(3)
_cell_length_c                   21.779(2)
_cell_measurement_reflns_used    9680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.893
_cell_measurement_theta_min      2.405
_cell_volume                     10662.7(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      99.93
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.979
_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  0.0195
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92615
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.935
_diffrn_reflns_theta_min         1.351
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0513 before and 0.0324 after correction. The Ratio of minimum to maximum transmission is 0.9214. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       prism
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.338
_exptl_crystal_size_min          0.318
_refine_diff_density_max         1.673
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1474
_refine_ls_number_reflns         25071
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0478P)^2^+13.2585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20712
_reflns_number_total             25071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03511g3.cif
_cod_data_source_block           mo_5886_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7701086--7701108.cif.'
_cod_original_cell_volume        10662.8(18)
_cod_database_code               7701096
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.883
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C110-C111 = C112-C107 = C108-C109
 1.39 with sigma of 0.02
 C110-C112
 2.4 with sigma of 0.04
 C111-C107
 2.4 with sigma of 0.04
 C112-C108
 2.4 with sigma of 0.04
 C107-C109
 2.4 with sigma of 0.04
 C108-C110
 2.4 with sigma of 0.04
3. Restrained planarity
 C107, C108, C109, C110, C111, C112, C113
 with sigma of 0.1
4. Rigid bond restraints
 C100, C101, C102, C103, C104, C105, C106
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C107, C108, C109, C110, C111, C112, C113
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1A, C1B, C1C, C1D, C1E, C1F, C121
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.08
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C121: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.08
Uanis(C113) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C107) \\sim Ueq,
Uanis(C112) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1F)=Sof(H1F)=Sof(C121)=Sof(H121)=
 Sof(C1B)=Sof(C1C)=Sof(H1C)=Sof(C1D)=Sof(H1D)=Sof(C1E)=Sof(H1E)=1-FVAR(1)
 Sof(C100)=Sof(H100)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=
 Sof(H103)=Sof(C104)=Sof(H104)=Sof(C105)=Sof(C106)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40),
  C42(H42), C43(H43), C45(H45), C46(H46), C84(H84), C85(H85), C86(H86),
 C87(H87), C88(H88), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94),
 C112(H112), C107(H107), C108(H108), C109(H109), C110(H110), C114(H114),
 C115(H115), C116(H116), C117(H117), C119(H119), C100(H100), C101(H101),
 C102(H102), C103(H103), C104(H104), C1F(H1F), C121(H121), C1C(H1C), C1D(H1D),
 C1E(H1E)
7.c Fitted hexagon refined as free rotating group:
 C112(C107,C108,C109,C110,C111), C100(C101,C102,C103,C104,C105), C1F(C121,C1B,
 C1C,C1D,C1E)
7.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C89(H89A,H89B,H89C), C96(H96A,H96B,H96C), C113(H11D,H11E,H11F),
 C120(H12D,H12E,H12F), C106(H10A,H10B,H10C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              67701
_shelx_fab_checksum              71997
_olex2_submission_special_instructions 'No special instructions were received'