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_7216069
_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         'C10 H36 N14 Ni3 O20 S4'
_chemical_formula_sum            'C10 H36 N14 Ni3 O20 S4'
_chemical_formula_weight         976.90
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.872(2)
_cell_angle_beta                 111.431(2)
_cell_angle_gamma                110.706(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1440(2)
_cell_length_b                   12.2530(2)
_cell_length_c                   13.0390(3)
_cell_measurement_reflns_used    524
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      3.59
_cell_volume                     1637.53(7)
_computing_cell_refinement       'HKL DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'HKL DENZO and SCALEPACK'
_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 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45507
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         3.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.064
_exptl_absorpt_correction_T_max  0.6830
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         7524
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                4541
_reflns_number_total             7524
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b505655a.txt
_cod_data_source_block           1
_cod_original_cell_volume        1637.52(5)
_cod_database_code               7216069