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_7008955
_publ_section_title
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 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_formula_sum            'C17 H30 F6 N5 Ni P S'
_chemical_formula_weight         540.20
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.10(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.202(3)
_cell_length_b                   24.771(7)
_cell_length_c                   16.585(5)
_cell_measurement_reflns_used    98
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      12.581
_cell_measurement_theta_min      4.565
_cell_volume                     4595(2)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  '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  0.0906
_diffrn_reflns_av_sigmaI/netI    0.1412
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11314
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        3.5
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.6394
_exptl_absorpt_correction_T_min  0.5764
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'deep green '
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         8055
_refine_ls_number_restraints     1287
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.2213
_reflns_number_gt                3971
_reflns_number_total             8055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907367a.txt
_cod_data_source_block           dsl05
_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:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7008955