Synthesis, X-ray characterization, DFT calculations and Hirshfeld surface analysis studies of carbohydrazone based on Zn(ii) complexes
Mahmoudi, Ghodrat; Bauzá, Antonio; Rodríguez-Diéguez, Antonio; Garczarek, Piotr; Kaminsky, Werner; Frontera, Antonio; CrystEngComm 18 (2016) 102–; doi:10.1039/C5CE01915J

data_7223306
_publ_section_title
;
 Synthesis, X-ray characterization, DFT calculations and Hirshfeld surface
 analysis studies of carbohydrazone based on Zn(ii) complexes
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              102
_journal_paper_doi               10.1039/C5CE01915J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C66 H64 Cl4 N24 O22 Zn4'
_chemical_formula_weight         1948.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-21 deposited with the CCDC.
2015-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.226(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7479(7)
_cell_length_b                   13.6207(7)
_cell_length_c                   44.742(2)
_cell_measurement_reflns_used    7454
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.57
_cell_measurement_theta_min      2.22
_cell_volume                     8292.0(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1231
_diffrn_reflns_av_sigmaI/netI    0.1549
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            158280
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         33.20
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.9230
_exptl_absorpt_correction_T_min  0.8541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Squeeze result sconsisten with 2 molecules of methanol solvent disordered
over multiple accessible voids in the asymmetric unit.  This is consistent
with the density map which showed partial occupancy of methanol is various
sites throughout the asymmetric unit.  The empirical formula was augmented
to include these removed molecules.

PLATON Reference : Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
                     Spek, A.L. (2009). Acta Cryst. D65, 148-155.
;
_refine_diff_density_max         2.603
_refine_diff_density_min         -1.819
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         31609
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                15737
_reflns_number_total             31609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01915j2.cif
_cod_data_source_block           grat012s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7223305--7223309.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7223306