1,2,4-Diazaphospholide Complexes of Barium: Mechanism of Formation and Crystallographic Characterization
Chengfu Pi; Li Wan; Weiping Liu; Zaifu Pan; Haoyu Wu; Yunhua Wang; Wenjun Zheng; Linhong Weng; Zhenxia Chen; Limin Wu; Inorganic Chemistry 48 (2009) 2967–2975; doi:10.1021/ic802157g

data_4301822
_publ_section_title
;
1,2,4-Diazaphospholide Complexes of Barium: Mechanism of Formation and
Crystallographic Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2967
_journal_page_last               2975
_journal_paper_doi               10.1021/ic802157g
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C16 H28 Ba N4 O6 P2'
_chemical_formula_weight         571.70
_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                75.072(8)
_cell_angle_beta                 73.752(7)
_cell_angle_gamma                74.300(8)
_cell_formula_units_Z            2
_cell_length_a                   9.980(7)
_cell_length_b                   10.186(7)
_cell_length_c                   13.325(9)
_cell_measurement_reflns_used    3727
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24899
_cell_measurement_theta_min      2.698
_cell_volume                     1227.5(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      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4983
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.8145
_exptl_absorpt_correction_T_min  0.7758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.834
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4185
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1283P)^2^+5.8602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2207
_refine_ls_wR_factor_ref         0.2247
_reflns_number_gt                3687
_reflns_number_total             4185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802157g_si_003.cif
_cod_data_source_block           f80522a
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1227.5(14)
_cod_database_code               4301822