Trimeric cyclamers: solution aggregation and high Z' crystals based on guest structure and basicity.
Kennedy, Stuart R.; Miquelot, Adeline; Aguilar, Juan A.; Steed, Jonathan W.; Chemical communications (Cambridge, England) 52 (2016) 11846–11849; doi:10.1039/c6cc06054d

data_7124984
_publ_section_title
;
 Trimeric cyclamers: solution aggregation and high Z' crystals based on
 guest structure and basicity.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11846
_journal_page_last               11849
_journal_paper_doi               10.1039/c6cc06054d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C12.2 H11.5 N2.7 O5.4'
_chemical_formula_weight         282.34
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-22 deposited with the CCDC.
2016-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.707(3)
_cell_length_b                   17.707(3)
_cell_length_c                   7.3732(10)
_cell_measurement_reflns_used    2853
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      1.58
_cell_volume                     2311.8(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Diamond I19'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            22865
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.310
_diffrn_reflns_theta_min         1.576
_diffrn_source                   'Diamond I19'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       needle
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.001
_platon_squeeze_details
;
From PLaton electron count of 358 per cell there should be 5.6 nitrobenzene
molecules per unit cell.
;
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 1007 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.7(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1042P)^2^+3.3608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2027
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2613
_reflns_number_total             2853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06054d2.cif
_cod_data_source_block           NBZSQZ
_cod_original_cell_volume        2311.8(7)
_cod_original_formula_sum        'C12.20 H11.50 N2.70 O5.40'
_cod_database_code               7124984
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              21841
_shelx_hkl_checksum              22035