Structural manipulation through selective substitution of hydrogen bonding groups: the supramolecular structures of bis(thiosemicarbazidato)nickel complexes
Burrows, Andrew D.; Harrington, Ross W.; Mahon, Mary F.; Teat, Simon J.; CrystEngComm 4 (2002) 539–; doi:10.1039/b208284e

data_7216586
_publ_section_title
;
 Structural manipulation through selective substitution of hydrogen
 bonding groups: the supramolecular structures of
 bis(thiosemicarbazidato)nickel complexes
;
_journal_issue                   89
_journal_name_full               CrystEngComm
_journal_page_first              539
_journal_paper_doi               10.1039/b208284e
_journal_volume                  4
_journal_year                    2002
_chemical_formula_sum            'C10 H24 N6 Ni S2'
_chemical_formula_weight         351.18
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   26.901(6)
_cell_length_b                   26.901(6)
_cell_length_c                   5.7535(12)
_cell_measurement_temperature    150(2)
_cell_volume                     3605.8(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker AXS diffractometer'
_diffrn_measurement_method       'Area detector'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6627
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         3.65
_exptl_absorpt_coefficient_mu    1.468
_exptl_absorpt_correction_T_max  0.8854
_exptl_absorpt_correction_T_min  0.2168
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1674
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0460
_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 
[1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
[\s^2^(Fo^2^)+0.0000+10.4875*P+(0.0377P)^2^+0.0000sin\q/\l] 
where P = 0.00000Fo^2^ + 1.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                1862
_reflns_number_total             1967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208284e.txt
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3605.8(13)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7216586