Formation of Cage Compounds Containing Boron, Phosphorus, and Transition Metal Atoms
Tuqiang Chen; Eileen N. Duesler; Robert T. Paine; Heinrich Nöth; Inorganic Chemistry 37 (1998) 490–495; doi:10.1021/ic970965s

data_4322637
_publ_section_title
;
 Formation of Cage Compounds Containing Boron, Phosphorus, and Transition
 Metal Atoms
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              490
_journal_page_last               495
_journal_paper_doi               10.1021/ic970965s
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C24 H58 B2 N2 P4 Pd'
_chemical_formula_weight         626.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Patterson map interpretation'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.72(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.212(4)
_cell_length_b                   10.225(1)
_cell_length_c                   17.406(2)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.38
_cell_measurement_theta_min      2.25
_cell_volume                     3426.6(9)
_computing_cell_refinement       'Siemens XSCANS, 1991'
_computing_data_collection       'Siemens XSCANS, 1991'
_computing_data_reduction        'Siemens XSCANS, 1991'
_computing_molecular_graphics    'Siemens SHELXTL-PC, 1990'
_computing_publication_material  'Siemens SHELXTL-PC, 1990'
_computing_structure_refinement  'Siemens SHELXTL-PC, 1990'
_computing_structure_solution    'Siemens SHELXTL-PC, 1990'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0962
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6188
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        8.73%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.9133
_exptl_absorpt_correction_T_min  0.8242
_exptl_absorpt_correction_type   'Semi-empirical \y-scans'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular chip'
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_obs      1.050
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_obs          0.0405
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(F)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0301
_refine_ls_wR_factor_obs         0.0273
_reflns_number_observed          2063
_reflns_number_total             3021
_reflns_observed_criterion       F>2sigma(F)
_cod_data_source_file            ic970965s_2.cif
_cod_data_source_block           rtp963
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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^(F)]' 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^(F)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3426.5(9)
_cod_database_code               4322637