Crystal structures and vibrational and solid-state (CPMAS) NMR spectroscopy of some bis(triphenylphosphine)silver(I) sulfate, selenate and phosphate systems
Bowmaker, Graham A.; Hanna, John V.; Rickard, Clifton E. F.; Lipton, Andrew S.; Journal of the Chemical Society, Dalton Transactions  (2001) 20–; doi:10.1039/b007796h

data_7010292
_publ_section_title
;
 Crystal structures and vibrational and solid-state (CPMAS) NMR
 spectroscopy of some bis(triphenylphosphine)silver(I) sulfate,
 selenate and phosphate systems
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              20
_journal_paper_doi               10.1039/b007796h
_journal_year                    2001
_chemical_formula_sum            'C36 H33 Ag O5 P2 Se'
_chemical_formula_weight         794.39
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.3870(10)
_cell_angle_beta                 91.6760(10)
_cell_angle_gamma                117.4040(10)
_cell_formula_units_Z            4
_cell_length_a                   12.5358(2)
_cell_length_b                   13.2580(2)
_cell_length_c                   24.5566(2)
_cell_measurement_reflns_used    7524
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     3460.39(9)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT  (Siemens, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 Sheldrick, (1997)'
_computing_structure_solution    'SHELXS Sheldrick, (1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'Area detector \w 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  0.0272
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32862
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         0.87
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  0.8028
_exptl_absorpt_correction_T_min  0.5240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.196
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_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         14255
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          1.010
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+15.3110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                11986
_reflns_number_total             14255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007796h.txt
_cod_data_source_block           gab9969
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+15.3110P] 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^)+(0.0139P)^2^+15.3110P] 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        3460.39(8)
_cod_database_code               7010292