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_4322638
_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            'C30 H66 B2 N2 P4 Pd'
_chemical_formula_weight         706.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6060(10)
_cell_length_b                   12.6180(10)
_cell_length_c                   24.221(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.21
_cell_measurement_theta_min      5.18
_cell_volume                     3852.7(6)
_computing_cell_refinement       'Siemens XSCANS, 1991'
_computing_data_collection       'Siemens XSCANS, 1991'
_computing_data_reduction        'Siemens XSCANS, 1991'
_computing_molecular_graphics    'Siemens SHELXTl/PC Version 5.0, 1994'
_computing_publication_material  'Siemens SHELXTl/PC Version 5.0, 1994'
_computing_structure_refinement  'Siemens SHELXTl/PC Version 5.0, 1994'
_computing_structure_solution    'Siemens SHELXTl/PC Version 5.0, 1994'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens Pr'
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.1935
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7582
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   'semi-empirical \y-scans'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'long rod'
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         6761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.224
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_obs          0.0396
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;  
 [0.00000+1.00000exp(5.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0100P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0792
_refine_ls_wR_factor_obs         0.0658
_reflns_number_observed          3372
_reflns_number_total             6761
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970965s_3.cif
_cod_data_source_block           rtp965
_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 
;
_cod_database_code               4322638
_cod_database_fobs_code          4322638