Formation of nickel-thiolate aggregates via reaction with CH2Cl2
Wang, Qiang; Marr, Andrew C.; Blake, Alexander J.; Wilson, Claire; Schr�der, Martin; Chemical Communications  (2003) 2776–; doi:10.1039/b309523a

data_7111307
_publ_section_title
;
 Formation of nickel-thiolate aggregates via reaction with CH2Cl2
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2776
_journal_paper_doi               10.1039/b309523a
_journal_year                    2003
_chemical_formula_moiety         'C92 H96 Cl2 Ni5 P4 S8, 4(C H2 Cl2)'
_chemical_formula_sum            'C96 H104 Cl10 Ni5 P4 S8'
_chemical_formula_weight         2286.20
_chemical_name_systematic
;
[Ni5Cl2(L1)4(dppe)2]
;
_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
'placed geometrically, Me from difference Fourier method'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier methods'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.446(2)
_cell_angle_beta                 82.054(2)
_cell_angle_gamma                66.885(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0330(7)
_cell_length_b                   13.1947(8)
_cell_length_c                   19.0517(12)
_cell_measurement_reflns_used    7162
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.4
_cell_volume                     2523.3(3)
_computing_cell_refinement       'SAINT (Bruker, 1999a)'
_computing_data_collection       'SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.045
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15902
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999b)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1178
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.84
_refine_diff_density_rms         0.10
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    'riding model, Me as rigid rotating group'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         11126
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+2.3725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                7928
_reflns_number_total             11126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309523asup1.cif
_cod_data_source_block           NIDPS2
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2523.3(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111307