[(5-Nitro-1,10-phenanthroline-<i>N</i>,<i>N</i>')(1,4,7-trithiacyclononane-<i>S</i>,<i>S</i>',<i>S</i>'')palladium(II)] Bis(hexafluorophosphate) Nitromethane Solvate
Blake, Alexander J.; Champness, Neil R.; Li, Wan-Sheung; Schröder, Martin; Acta Crystallographica Section C 54 (1998) IUC9800071–; doi:10.1107/S0108270198099156

data_2008009
_publ_section_title
;[(5-Nitro-1,10-phenanthroline-<i>N</i>,<i>N</i>')(1,4,7-trithiacyclononane-<i>S</i>,<i>S</i>',<i>S</i>'')palladium(II)]
 Bis(hexafluorophosphate) Nitromethane Solvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800071
_journal_paper_doi               10.1107/S0108270198099156
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac
'[Pd (C12 H7 N3 O2) (C6 H12 S3)] (P F6)2, C H3 N O2'
_chemical_formula_moiety         'C18 H19 N3 O2 Pd S3 2+, 2 P F6 -, C H3 N O2'
_chemical_formula_sum            'C19 H22 F12 N4 O4 P2 Pd S3'
_chemical_formula_weight         862.93
_chemical_name_common            ([9]aneS3)(5-NO2-phen)Pd](PF6)2.MeNO2
_chemical_name_systematic
;[(5-Nitro-1,10-phenanthroline)(1,4,7-trithiacyclononane-S,S',S")palladium(II)]
Bis(hexafluorophosphate)
 Nitromethane Solvate
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.49(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.541(4)
_cell_length_b                   13.177(4)
_cell_length_c                   17.060(4)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      14.45
_cell_measurement_theta_min      11.75
_cell_volume                     3010.7(15)
_computing_cell_refinement       STADI-4
_computing_data_collection       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       \w/\q
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4216
_diffrn_reflns_theta_full        23.23
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        9.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 1996b)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    'H atoms: riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         4192
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.121
_refine_ls_R_factor_gt           0.077
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0395P)^2^+47.27P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.190
_reflns_number_gt                2971
_reflns_number_total             4192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            qa0064.cif
_cod_data_source_block           qa0064
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_refinement_flags' value 'r' changed to 'R' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

'_atom_site_refinement_flags' value 'd' changed to 'D'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'NO' changed to 'no'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).

'_geom_angle_publ_flag' value 'NO' changed to 'no' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).

'_geom_torsion_publ_flag' value 'NO' changed to 'no'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_atom_site_refinement_flags' value 'Pd' changed to 'PD' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (6 times).

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0395P)^2^+47.27P] 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^)+(0.0395P)^2^+47.27P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2008009