Solvent-induced 1,3-N,S- vs. 1,5-S,S′-coordination in the NiII complex [Ni{p-Me2NC6H4NHC(S)NP(S)(OiPr)2}2]
Babashkina, Maria G.; Safin, Damir A.; Srebro, Monika; Kubisiak, Piotr; Mitoraj, Mariusz P.; Bolte, Michael; Garcia, Yann; CrystEngComm 13 (2011) 5321–; doi:10.1039/c1ce05387f

data_7206407
_publ_section_title
;
 Solvent-induced 1,3-N,S- vs. 1,5-S,S&#x2032;-coordination in the NiII
 complex [Ni{p-Me2NC6H4NHC(S)NP(S)(OiPr)2}2]
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              5321
_journal_paper_doi               10.1039/c1ce05387f
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C30 H50 N6 Ni O4 P2 S4'
_chemical_formula_sum            'C30 H50 N6 Ni O4 P2 S4'
_chemical_formula_weight         807.65
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.796(2)
_cell_angle_beta                 73.261(2)
_cell_angle_gamma                72.496(2)
_cell_formula_units_Z            6
_cell_length_a                   15.0369(5)
_cell_length_b                   17.5722(6)
_cell_length_c                   24.6552(8)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     5925.1(4)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens CCD three-circle diffractometer'
_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  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            111312
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         0.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.9004
_exptl_absorpt_correction_T_min  0.7234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1281
_refine_ls_number_reflns         21625
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+3.5487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                13151
_reflns_number_total             21625
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1ce05387f.txt
_cod_data_source_block           safin85
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        5925.1(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7206407