The structural influence of ligand coordination and hydrogen bonding capabilities in the crystal engineering of metal thiosemicarbazide compounds with malonate
Burrows, Andrew D.; Harrington, Ross W.; Mahon, Mary F.; Teat, Simon J.; CrystEngComm 7 (2005) 388–; doi:10.1039/b505655a

data_7216071
_publ_section_title
;
 The structural influence of ligand coordination and hydrogen bonding
 capabilities in the crystal engineering of metal thiosemicarbazide
 compounds with malonate
;
_journal_issue                   64
_journal_name_full               CrystEngComm
_journal_page_first              388
_journal_paper_doi               10.1039/b505655a
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         'C12 H34 N10 Ni O9 S3'
_chemical_formula_sum            'C12 H34 N10 Ni O9 S3'
_chemical_formula_weight         617.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.868(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.711(2)
_cell_length_b                   10.2151(15)
_cell_length_c                   18.702(3)
_cell_measurement_reflns_used    34278
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.28
_cell_volume                     2600.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69410
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33308
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.27
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.9793
_exptl_absorpt_correction_T_min  0.8338
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0319P)^2^+1.1527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                6145
_reflns_number_total             7138
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b505655a.txt
_cod_data_source_block           3
_cod_original_cell_volume        2600.5(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7216071