Chelate effects in sulfate binding by amide/urea-based ligands.
Jia, Chuandong; Wang, Qi-Qiang; Begum, Rowshan Ara; Day, Victor W.; Bowman-James, Kristin; Organic & biomolecular chemistry 13 (2015) 6953–6957; doi:10.1039/c5ob00618j

data_7157216
_publ_section_title
;
 Chelate effects in sulfate binding by amide/urea-based ligands.
;
_journal_issue                   25
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6953
_journal_page_last               6957
_journal_paper_doi               10.1039/c5ob00618j
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C43 H97 N7 O6 S'
_chemical_formula_weight         840.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-02-26 deposited with the CCDC.
2015-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.5590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1475(3)
_cell_length_b                   22.3413(7)
_cell_length_c                   12.6753(4)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.29
_cell_measurement_theta_min      4.06
_cell_volume                     2546.55(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21070
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         69.402
_diffrn_reflns_theta_min         3.547
_diffrn_source                   'Bruker MicroStar microfocus rotating anode'
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
; 
 Flack x determined using 3278 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.054(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8045
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.3963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.711
_reflns_Friedel_fraction_full    0.763
_reflns_Friedel_fraction_max     0.722
_reflns_number_gt                7958
_reflns_number_total             8045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob00618j2.cif
_cod_data_source_block           q66b
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7157216
_shelx_estimated_absorpt_t_min   0.706
_shelx_estimated_absorpt_t_max   0.937
_shelxl_version_number           2013-4
_shelx_res_checksum              25316