Crystal structure of bis(μ-thiocyanato-N,S)bis[aqua-(3-methylbenzo- 15-crown-5)sodium]bis(thiocyanato-S)-palladium(II), [Na(C~15~H~22~O~5~) (H~2~O)]~2~[Pd(SCN)~4~]
M.-J. Niu; D.-C. Li; J.-M. Dou; D.-Q. Wang; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 185–187; doi:

data_8101729
_publ_section_title
;
Crystal structure of bis(\m-thiocyanato-N,S)bis[aqua-(3-methylbenzo-
15-crown-5)sodium]bis(thiocyanato-S)-palladium(II), [Na(C~15~H~22~O~5~)
(H~2~O)]~2~[Pd(SCN)~4~]
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              185
_journal_page_last               187
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         '[Pd{Na[(o-MeB15C5)(H~2~O)]}~2~(SCN)~4~]'
_chemical_formula_sum            'C34 H48 N4 Na2 O12 Pd S4'
_chemical_formula_weight         985.38
_chemical_melting_point          356.1(10)
_chemical_name_common            Pd{Na[(C~15~H~22~O~5~)(H~2~O)]}~2~(SCN)~4~
_chemical_name_systematic
; 
bis(\m-thiocyanato-N,S)bis[aqua-(3-methylbenzo-15-crown-5)sodium]bis
(thiocyanato-S)palladium(II)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.47(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.879(16)
_cell_length_b                   16.90(2)
_cell_length_c                   13.211(18)
_cell_measurement_reflns_used    2456
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.095
_cell_measurement_theta_min      3.124
_cell_volume                     2276(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11214
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.7710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'salmon pink'
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4021
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                2409
_reflns_number_total             4021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1469.cff
_cod_data_source_block           040103b
_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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '82-84 C' was changed to '356.1(10)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2275(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               8101729