Chlorides, Oxochlorides, and Oxoacids of 1,8-Diphosphanaphthalene: A System with Imposed Close P...P Interaction
Petr Kilian; Heather L. Milton; Alexandra M. Z. Slawin; J. Derek Woollins; Inorganic Chemistry 43 (2004) 2252–2260; doi:10.1021/ic035364h

data_4310806
_publ_section_title
;
 Chlorides, Oxochlorides, and Oxoacids of 1,8-Diphosphanaphthalene: A
 System with Imposed Close P...P Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2252
_journal_page_last               2260
_journal_paper_doi               10.1021/ic035364h
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C20 H12 Cs2 O4 P4.2[C H4 O]'
_chemical_formula_sum            'C22 H20 Cs2 O6 P4'
_chemical_formula_weight         770.08
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic        ?
_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                109.050(11)
_cell_angle_beta                 90.524(12)
_cell_angle_gamma                90.620(13)
_cell_formula_units_Z            2
_cell_length_a                   7.157(5)
_cell_length_b                   12.363(9)
_cell_length_c                   14.690(10)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      12
_cell_volume                     1228.4(15)
_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      125(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6086
_diffrn_reflns_theta_max         23.43
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    3.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.626939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_ls_extinction_coef       0.0038(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    RIDING
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                2578
_reflns_number_total             3396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035364hsi20031201_043220_3.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to
'/home/adriana/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 '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' 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 

Replacing value '-' with '?' for the following tags 
'_chemical_name_common', '_chemical_name_systematic', 
'_diffrn_standards_decay_%', '_diffrn_standards_interval_count', 
'_diffrn_standards_interval_time', '_diffrn_standards_number',
'_exptl_absorpt_process_details'.

Antanas Vaitkus, 2015-02-20
;
_cod_original_cell_volume        1228.6(15)
_cod_database_code               4310806