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_7701093
_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
'C39 H45 N4 O Pd, C51 H16 B2 F30 N3 O, C H2 Cl2'
_chemical_formula_sum            'C91 H63 B2 Cl2 F30 N7 O2 Pd'
_chemical_formula_weight         2055.40
_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             2019-05-24
_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                115.371(3)
_cell_angle_beta                 106.919(3)
_cell_angle_gamma                99.963(4)
_cell_formula_units_Z            2
_cell_length_a                   15.857(3)
_cell_length_b                   19.087(4)
_cell_length_c                   19.142(4)
_cell_measurement_reflns_used    9096
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.852
_cell_measurement_theta_min      2.384
_cell_volume                     4701.8(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0172
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83372
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.922
_diffrn_reflns_theta_min         1.258
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0337 before and 0.0285 after correction. The Ratio of minimum to maximum transmission is 0.9438. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.185
_refine_diff_density_max         2.062
_refine_diff_density_min         -2.391
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         22304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0557P)^2^+7.0976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20376
_reflns_number_total             22304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03511g3.cif
_cod_data_source_block           mo_6038_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7701086--7701108.cif.'
_cod_original_cell_volume        4701.8(16)
_cod_database_code               7701093
_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.a Ternary CH refined with riding coordinates:
 C37(H37), C25(H25), C22(H22), C34(H34)
2.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C53(H53A,H53B), C52(H52A,H52B), C50(H50A,H50B), C51(H51A,
 H51B), C91(H91A,H91B)
2.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C41(H41), C40(H40), C48(H48), C47(H47), C14(H14), C15(H15), C8(H8),
 C30(H30), C45(H45), C10(H10), C9(H9), C20(H20), C18(H18), C32(H32), C19(H19),
 C3(H3), C31(H31), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C38(H38A,H38B,
 H38C), C26(H26A,H26B,H26C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C12(H12A,
 H12B,H12C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              21220
_shelx_fab_checksum              49835
_olex2_submission_special_instructions 'No special instructions were received'