Experiences with applications of macromolecular tools in supramolecular crystallography
Wierzbicki, Michał; Gilski, Mirosław; Rissanen, Kari; Jaskólski, Mariusz; Szumna, Agnieszka; CrystEngComm 16 (2014) 3773–; doi:10.1039/c3ce42288g

data_7214355
_publ_section_title
;
 Experiences with applications of macromolecular tools in supramolecular
 crystallography
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3773
_journal_paper_doi               10.1039/c3ce42288g
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_formula_sum            'C133.5 H197 N8 O37.5'
_chemical_formula_weight         2513.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7322(4)
_cell_length_b                   24.0717(7)
_cell_length_c                   41.3778(12)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      58.20
_cell_measurement_theta_min      3.36
_cell_volume                     15669.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    PHASER
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.774
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_Laue_measured_fraction_full 0.774
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            33459
_diffrn_reflns_point_group_measured_fraction_full 0.722
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.988
_diffrn_reflns_theta_min         3.005
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.9490
_exptl_absorpt_correction_T_min  0.7634
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_description       prism
_exptl_crystal_F_000             5416
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 6997 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.11(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1683
_refine_ls_number_reflns         20472
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1112P)^2^+15.4547P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2010
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_full    0.661
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                18362
_reflns_number_total             20472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce42288g.txt
_cod_data_source_block           Comp1_KR
_cod_original_formula_sum        'C133.50 H197 N8 O37.50'
_cod_database_code               7214355
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.954