Sandwich phosphate complexes of macrocyclic tris(urea) ligands and their rotation around the anion
Liguo Ji; Zaiwen Yang; Yanxia Zhao; Meng Sun; Liping Cao; Xiao-Juan Yang; Yao-Yu Wang; Biao Wu; Chem.Commun. 52 (2016) 7310–; doi:

data_7118996
_publ_section_title
;
 Sandwich phosphate complexes of macrocyclic tris(urea) ligands and their
 rotation around the anion
;
_journal_name_full               Chem.Commun.
_journal_page_first              7310
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C51 H78 Cl N9 O14'
_chemical_formula_weight         1076.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-26 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.732(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.572(5)
_cell_length_b                   34.162(8)
_cell_length_c                   8.774(2)
_cell_measurement_temperature    173(2)
_cell_volume                     5548(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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0783
_diffrn_reflns_av_sigmaI/netI    0.1053
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27129
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.9552
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.772
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         9855
_refine_ls_number_restraints     1032
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.2653
_refine_ls_R_factor_gt           0.1890
_refine_ls_shift/su_max          0.006
_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^+93.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3684
_refine_ls_wR_factor_ref         0.4077
_reflns_number_gt                5637
_reflns_number_total             9855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc03144g2.cif
_cod_data_source_block           07
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               7118996