Ci-symmetry, [2 × 2] grid, square copper complex with the N4,N5-bis(4-fluorophenyl)-1H-imidazole-4,5-dicarboxamide ligand: structure, catecholase activity, magnetic properties and DFT calculations
Parween, Arfa; Naskar, Sumita; Mota, Antonio J.; Espinosa, Arturo; Chattopadhyay, Shyamal Kumar; Riviere, Eric; Lewis, William; Naskar, Subhendu; New J. Chem. 41 (2017) 11750–11758; doi:10.1039/C7NJ01667K

data_7056499
_publ_section_title
;
 Ci-symmetry, [2 \\times 2] grid, square copper complex with the
 N4,N5-bis(4-fluorophenyl)-1H-imidazole-4,5-dicarboxamide ligand:
 structure, catecholase activity, magnetic properties and DFT calculations
;
_journal_issue                   20
_journal_name_full               'New J. Chem.'
_journal_page_first              11750
_journal_page_last               11758
_journal_paper_doi               10.1039/C7NJ01667K
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C80 H68 Cu4 F8 N20 O12'
_chemical_formula_sum            'C80 H68 Cu4 F8 N20 O12'
_chemical_formula_weight         1907.70
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2017-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                91.449(7)
_cell_angle_beta                 98.769(6)
_cell_angle_gamma                113.892(9)
_cell_formula_units_Z            1
_cell_length_a                   10.1601(8)
_cell_length_b                   12.4693(14)
_cell_length_c                   17.1951(11)
_cell_measurement_reflns_used    6549
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.4370
_cell_measurement_theta_min      3.8780
_cell_volume                     1959.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega   66.00  102.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000   90.0000 18

  2 omega   62.00   96.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000    0.0000 17

  3 omega   50.00  134.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  -90.0000 42

  4 omega   94.00  120.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  -30.0000 13

  5 omega   43.00   89.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -30.0000 23

  6 omega  116.00  160.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000 -120.0000 22

  7 omega  136.00  164.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  -30.0000 14

  8 omega  114.00  158.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 22

  9 omega   83.00  165.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000    0.0000 41

 10 omega  149.00  175.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000  -90.0000 13

 11 omega   96.00  132.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000  -90.0000 18

 12 omega   83.00  117.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  -30.0000 17

 13 omega   42.00   92.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000   90.0000 25

 14 omega   41.00  121.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  150.0000 40

 15 omega   38.00   64.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  -30.0000 13

 16 omega   31.00  103.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000 -150.0000 36

 17 omega   36.00   90.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -180.0000 27

 18 omega  -40.00  -14.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 13

 19 omega  -25.00   65.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6804  -57.0000  150.0000 45

 20 omega  -67.00   29.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   77.0000   60.0000 48

 21 omega    4.00   34.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 15

 22 omega -103.00  -13.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -77.0000  -60.0000 45
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.1070769000
_diffrn_orient_matrix_UB_12      -0.0254125000
_diffrn_orient_matrix_UB_13      0.0623232000
_diffrn_orient_matrix_UB_21      0.0734424000
_diffrn_orient_matrix_UB_22      0.1312263000
_diffrn_orient_matrix_UB_23      0.0317047000
_diffrn_orient_matrix_UB_31      -0.1074386000
_diffrn_orient_matrix_UB_32      -0.0237494000
_diffrn_orient_matrix_UB_33      0.0583566000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14052
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.612
_diffrn_reflns_theta_min         3.895
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    2.052
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.3267
_exptl_crystal_size_mid          0.1147
_exptl_crystal_size_min          0.0837
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.062
_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     563
_refine_ls_number_reflns         7708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0475P)^2^+0.9682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6573
_reflns_number_total             7708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01667k2.cif
_cod_data_source_block           snwlll
_cod_database_code               7056499
_nottingham_internal_coll_name   SNWLLL
_nottingham_internal_coll_number 14539
_nottingham_internal_coll_client SN/WL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '3.0000, 2.0000'
_nottingham_internal_coll_frame_width 2.0000
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   01/04/2015
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 27/05/2015
_nottingham_internal_process_user pczwl
_nottingham_internal_solution_date 27/5/2015
_nottingham_internal_solution_user pczwl
_nottingham_internal_refinement_date 3/6/2015
_nottingham_internal_refinement_user pczwl
_nottingham_internal_validation_date 3/6/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 3/6/2015
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C80 H68 F8 N20 O12 Cu4'
_chemical_oxdiff_usercomment
'SNWLLL #14539 GVB-484 on micromount in fomblin film for SN/WL'
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C11(H11), C13(H13), C14(H14), N18(H18), C20(H20), C21(H21),
 C23(H23), C24(H24), C27(H27), C35(H35), C36(H36), C38(H38), C39(H39), N43(H43),
  C45(H45), C46(H46), C48(H48), C49(H49), C52(H52), C57(H57)
2.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C)
;
_shelx_res_checksum              47268
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'