Hydrogen bonding in coordinated thiosemicarbazones: ammine[2-hydroxy-1-naphthaldehyde 4-methylthiosemicarbazonato]nickel(II)
Valdés Martínez, Jesús; Hernández-Ortega, Simón; Bautista Jimenez, Victor; Acta Crystallographica Section E 60 (2004) m42–m44; doi:10.1107/S1600536803027971

data_2203075
_publ_section_title
;
 Hydrogen bonding in coordinated thiosemicarbazones:
 ammine[2-hydroxy-1-naphthaldehyde
 4-methylthiosemicarbazonato]nickel(II)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m42
_journal_page_last               m44
_journal_paper_doi               10.1107/S1600536803027971
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (C13 H11 N3 O S) (N H3)]'
_chemical_formula_moiety         'C13 H14 N4 Ni O S'
_chemical_formula_sum            'C13 H14 N4 Ni O S'
_chemical_formula_weight         333.05
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.345(4)
_cell_length_b                   5.3870(10)
_cell_length_c                   11.787(2)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      12.17
_cell_measurement_theta_min      1.93
_cell_volume                     1355.3(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4/PC'
_diffrn_measurement_method       \w
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3374
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        >2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  0.9398
_exptl_absorpt_correction_T_min  0.7831
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(SHELXTL/PC; Sheldrick 1997)'
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Laminar
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.411
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0344
_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^)+(0.04P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                1737
_reflns_number_total             2388
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6143.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2203075
_cod_database_fobs_code          2203075