Halide ion-driven self-assembly of Zn(ii) compounds derived from an asymmetrical hydrazone building block: a combined experimental and theoretical study
Mahmoudi, Ghodrat; Afkhami, Farhad Akbari; Jena, Himanshu Sekhar; Nematollahi, Parisa; Esrafili, Mehdi D.; Garczarek, Piotr; Van Hecke, Kristof; Servati Gargari, Masoumeh; Kirillov, Alexander M.; New J. Chem. 40 (2016) 10116–; doi:10.1039/C6NJ01534D

data_7055825
_publ_section_title
;
 Halide ion-driven self-assembly of Zn(ii) compounds derived from an
 asymmetrical hydrazone building block: a combined experimental and
 theoretical study
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              10116
_journal_paper_doi               10.1039/C6NJ01534D
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C56 H60 Cl8 N12 O12 Zn4'
_chemical_formula_sum            'C56 H60 Cl8 N12 O12 Zn4'
_chemical_formula_weight         1638.31
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-22
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_audit_update_record
;
2016-10-10 deposited with the CCDC.
2016-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.0619(6)
_cell_length_b                   22.0619(6)
_cell_length_c                   7.3434(4)
_cell_measurement_reflns_used    2692
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.6570
_cell_measurement_theta_min      2.8190
_cell_volume                     3574.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_details
;
  1 omega    2.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9298  -32.0000 -126.0000 66

  2 omega  -80.00   24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   95.0000  157.0000 104

  3 omega   54.00   84.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -32.0000  -32.0000 30

  4 omega   33.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -95.0000 -132.0000 65

  5 omega   43.00   78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -32.0000 -126.0000 35

  6 omega  -43.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9298  125.0000   60.0000 26

  7 omega  -93.00  -68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9298  125.0000   60.0000 25

  8 omega -123.00  -83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000 -150.0000 40

  9 omega   38.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -15.0000  120.0000 55

 10 omega   56.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000 -180.0000 43

 11 omega   70.00   96.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000  -60.0000 26

 12 omega  113.00  154.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -15.0000  120.0000 41

 13 omega   58.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000    0.0000 31

 14 omega   36.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000   90.0000 62
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0655510000
_diffrn_orient_matrix_UB_12      0.0200971000
_diffrn_orient_matrix_UB_13      -0.0398986000
_diffrn_orient_matrix_UB_21      -0.0193812000
_diffrn_orient_matrix_UB_22      -0.0209225000
_diffrn_orient_matrix_UB_23      0.1917255000
_diffrn_orient_matrix_UB_31      0.0145043000
_diffrn_orient_matrix_UB_32      0.0634416000
_diffrn_orient_matrix_UB_33      0.0754102000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7101
_diffrn_reflns_theta_full        75.30
_diffrn_reflns_theta_max         75.30
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.805
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1664.0
_exptl_crystal_size_max          0.1472
_exptl_crystal_size_mid          0.0537
_exptl_crystal_size_min          0.0457
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1960
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+1.0285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                1605
_reflns_number_total             1960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj01534d2.cif
_cod_data_source_block           fa005_rt
_cod_depositor_comments
'Adding full bibliography for 7055823--7055825.cif.'
_cod_original_cell_volume        3574.2(3)
_cod_database_code               7055825
_chemical_oxdiff_formula         'C56 H60 Cl8 N12 O12 Zn4'
_reflns_odcompleteness_completeness 100.00
_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 O(H) groups
2. Restrained distances
 O2-H2B
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 N2(H2A)
;
_shelx_res_checksum              98654
_shelx_fab_checksum              59994
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'