Completion of the Series of M2(hpp)4Cl2 Compounds from W to Pt: The W, Os, and Pt Compounds
Rodolphe Clérac; F. Albert Cotton; Lee M. Daniels; James P. Donahue; Carlos A. Murillo; Daren J. Timmons; Inorganic Chemistry 39 (2000) 2581–2584; doi:10.1021/ic991370v

data_4321042
_publ_section_title
;
 Completion of the Series of M2(hpp)4Cl2 Compounds from W to Pt: The W,
 Os, and Pt Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2581
_journal_page_last               2584
_journal_paper_doi               10.1021/ic991370v
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'W2 (C7 H12 N3)4 Cl2'
_chemical_formula_structural     W2(C7H12N3)4Cl2
_chemical_formula_sum            'C28 H48 Cl2 N12 W2'
_chemical_formula_weight         991.38
_chemical_melting_point          ?
_chemical_name_systematic
;
 [tetrakis(1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]
 pyrimidinate)ditungsten(III)]dichloride
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.949(2)
_cell_length_b                   9.949(2)
_cell_length_c                   15.841(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      6.75
_cell_volume                     1568.0(5)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP (SIEMENS, 1996)'
_computing_publication_material  'CIFTAB (SHELDRICK, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3203
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.42
_diffrn_standards_number         'None (area detector data)'
_exptl_absorpt_coefficient_mu    7.543
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.507
_exptl_absorpt_correction_type   'symmetry-related measurements'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.884
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.277
_refine_ls_goodness_of_fit_obs   1.282
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         542
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.266
_refine_ls_restrained_S_obs      1.271
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_obs          0.0529
_refine_ls_shift/esd_max         -0.047
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+90.0723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1139
_refine_ls_wR_factor_obs         0.1118
_reflns_number_observed          519
_reflns_number_total             542
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991370v_2.cif
_cod_data_source_block           W2(hpp)4Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_geom_bond_publ_flag' value
'N' changed to 'n' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (14
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (3 times).

'_geom_angle_publ_flag'
value 'Y' changed to 'y' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (27 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+90.0723P] 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^)+(0.0118P)^2^+90.0723P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1568.2(5)
_cod_database_code               4321042