Synthesis, characterization and crystal structures of the first pentacoordinate nickel(II) complexes containing N,S-donor ligands
M. Dolores Santana; Gabriel García; Antonio Rufete; M. Carmen Ramírez de Arellano; Gregorio López; J. Chem. Soc., Dalton Trans.  (2000) 619–625; doi:10.1039/a907367a

data_7008956
_publ_section_title
;
 Synthesis, characterization and crystal structures of the first
 pentacoordinate nickel(II) complexes containing N,S-donor ligands
;
_journal_issue                   4
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              619
_journal_page_last               625
_journal_paper_doi               10.1039/a907367a
_journal_year                    2000
_chemical_compound_source        'slow evaporation acetone solution'
_chemical_formula_sum            'C20 H32 F6 N5 Ni P S'
_chemical_formula_weight         578.25
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.728(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.938(2)
_cell_length_b                   14.318(2)
_cell_length_c                   15.938(2)
_cell_measurement_reflns_used    73
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.28
_cell_measurement_theta_min      3.700
_cell_volume                     2493.2(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.1122
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4797
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        2.04
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   'Psi scans'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.904
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    'NH free, rigid methyls others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4373
_refine_ls_number_restraints     598
_refine_ls_restrained_S_all      0.959
_refine_ls_restrained_S_obs      1.139
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_obs          0.0673
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2004
_refine_ls_wR_factor_obs         0.1707
_reflns_number_observed          2268
_reflns_number_total             4373
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a907367a.txt
_cod_data_source_block           dsl02
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2493.2(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7008956