Tris Chelating Phosphate Complexes of Bis(thio)urea Ligands
Rui Li; Yanxia Zhao; Shaoguang Li; Peiju Yang; Xiaojuan Huang; Xiao-Juan Yang; Biao Wu; Inorganic Chemistry 52 (2013) 5851–5860; doi:10.1021/ic3028012

data_4334831
_publ_contact_author_address
; Lanzhou Institute of Chemical Physics, 
Chinese Academy of Sciences, Lanzhou 730000, P. R. China
;
_publ_contact_author_email       yangxj@lzb.ac.cn
_publ_contact_author_fax         +86-931-4968286
_publ_contact_author_name        'Xiao-Juan, Yang'
_publ_contact_author_phone       +86-931-4968286
_publ_section_title
;
 Tris Chelating Phosphate Complexes of Bis(thio)urea Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5851
_journal_page_last               5860
_journal_paper_doi               10.1021/ic3028012
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C23 H19 N6 O8 S'
_chemical_formula_weight         539.50
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.433(2)
_cell_length_b                   20.900(11)
_cell_length_c                   30.555(16)
_cell_measurement_temperature    153(2)
_cell_volume                     2831(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w scan'
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            18803
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.9673
_exptl_absorpt_correction_T_min  0.9593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.5(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0000P)^2^+12.8060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2065
_refine_ls_wR_factor_ref         0.2186
_reflns_number_gt                3447
_reflns_number_total             4996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3028012_si_002_1.cif
_cod_data_source_block           L1
_cod_original_cell_volume        2831(3)
_cod_database_code               4334831