[1,2-Bis(diphenylphosphino)ethane-<i>P</i>,<i>P</i>'](4-morpholinecarbodithioato-<i>S</i>,<i>S</i>')nickel(II) Perchlorate Dichloromethane Solvate
Akilan, R.; Sivakumar, K.; Venkatachalam, V.; Ramalingam, K.; Chinnakali, K.; Fun, H.-K.; Acta Crystallographica Section C 51 (1995) 368–370; doi:10.1107/S010827019401070X

data_2003276
_publ_section_title
;[1,2-Bis(diphenylphosphino)ethane-<i>P</i>,<i>P</i>'](4-morpholinecarbodithioato-<i>S</i>,<i>S</i>')nickel(II)
 Perchlorate Dichloromethane Solvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              368
_journal_page_last               370
_journal_paper_doi               10.1107/S010827019401070X
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
;The preparation of the title compound was accomplished by established
 procedures
(Ramalingam, Aravamudan, Seshasayee & Subramanyam,
 1984;
Ramalingam, Aravamudan & Seshasayee, 1987). The parent
 dithiocarbamato
complex was prepared from morpholinium morpholine
 4-carbodithioate and
nickel chloride (Aravamudan, Brown & Venkappayya,
 1971).
Single crystals were obtained from
dichloromethane solution by slow
 evaporation at room temperature.
;
_chemical_formula_moiety         'C31 H32 N Ni O P2 S2 , CH2 Cl2 , Cl O4'
_chemical_formula_sum            'C32 H34 Cl3 N Ni O5 P2 S2'
_chemical_formula_weight         803.72
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.16(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.456(2)
_cell_length_b                   22.745(4)
_cell_length_c                   16.707(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      8
_cell_volume                     3587.8(12)
_computing_cell_refinement       'XSCANS (Siemens, 1991)'
_computing_data_collection       'XSCANS (Siemens, 1991)'
_computing_data_reduction        'XSCANS (Siemens, 1991)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL93
_computing_structure_refinement  SHELXL93
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4 four-circle'
_diffrn_measurement_method       '\q-2\q 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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8522
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Needles
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.869
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_obs          0.0510
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^) + (0.0621P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1306
_refine_ls_wR_factor_obs         0.1073
_reflns_number_observed          3962
_reflns_number_total             8245
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            li1125.cif
_cod_data_source_block           rams2
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'No' 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_sg_symbol_H-M      'P 21/c'
_cod_database_code               2003276