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_7055823
_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         'C26 H22 I2 N6 O4 Zn, 2(C H4 O)'
_chemical_formula_sum            'C28 H30 I2 N6 O6 Zn'
_chemical_formula_weight         865.77
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-17
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.03.22 svn.r2654, GUI svn.r4446)
;
_audit_update_record
;
2015-01-07 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            4
_cell_length_a                   7.81700(19)
_cell_length_b                   13.0929(4)
_cell_length_c                   30.6293(9)
_cell_measurement_reflns_used    2784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8540
_cell_measurement_theta_min      5.7750
_cell_volume                     3134.82(15)
_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      100(2)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9994
_diffrn_measurement_details
;
  1 omega  -67.00   11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   95.0000  -54.0000 78

  2 omega   34.00   70.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316 -115.0000  158.0000 36

  3 omega  101.00  175.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   95.0000  -54.0000 74

  4 omega   33.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -31.0000  144.0000 40

  5 omega  -34.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   38.0000 -150.0000 56

  6 omega   37.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798 -125.0000  -90.0000 60

  7 omega -125.00  -91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000   90.0000 34

  8 omega   47.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000 -180.0000 51

  9 omega   39.00   74.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000  -30.0000 35

 10 omega   30.00   99.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -95.0000   15.0000 69

 11 omega   39.00   89.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000   30.0000 50

 12 omega   59.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000 -150.0000 28

 13 omega   34.00   60.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000    0.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0554806000
_diffrn_orient_matrix_UB_12      0.0356183000
_diffrn_orient_matrix_UB_13      -0.0458028000
_diffrn_orient_matrix_UB_21      0.0553031000
_diffrn_orient_matrix_UB_22      0.1036576000
_diffrn_orient_matrix_UB_23      0.0191348000
_diffrn_orient_matrix_UB_31      0.1808197000
_diffrn_orient_matrix_UB_32      -0.0427330000
_diffrn_orient_matrix_UB_33      0.0081982000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            10924
_diffrn_reflns_theta_full        70.07
_diffrn_reflns_theta_max         70.07
_diffrn_reflns_theta_min         5.78
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.982
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.986
_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    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.1177
_exptl_crystal_size_mid          0.0606
_exptl_crystal_size_min          0.0551
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2959
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                2334
_reflns_number_total             2959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj01534d2.cif
_cod_data_source_block           fa002
_cod_depositor_comments
'Adding full bibliography for 7055823--7055825.cif.'
_cod_database_code               7055823
_chemical_oxdiff_formula         'C24 H15 I1 N3 O3 Zn'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2. Restrained distances
 H2A-N2
 0.88 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)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2B), O3(H3)
;