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_7118997
_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 H68 I2 N10 O10'
_chemical_formula_weight         1234.95
_chemical_name_systematic
; 
 ? 
;
_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
_audit_update_record
;
2016-02-26 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                71.072(2)
_cell_angle_beta                 78.8600(10)
_cell_angle_gamma                70.582(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2750(16)
_cell_length_b                   13.0629(17)
_cell_length_c                   19.863(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2828.3(7)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17824
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.7990
_exptl_absorpt_correction_T_min  0.7578
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.243
_refine_diff_density_min         -4.472
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9664
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+30.5449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                8358
_reflns_number_total             9664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc03144g2.cif
_cod_data_source_block           08
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to 'constr'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 4609 2016-04-01 06:22:49Z antanas 
;
_cod_original_cell_volume        2828.3(6)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7118997