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_7124986
_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            'C8 H10 N2 O5'
_chemical_formula_weight         214.18
_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'
_atom_sites_solution_hydrogens   mixed
_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            4
_cell_length_a                   4.5426(19)
_cell_length_b                   10.729(5)
_cell_length_c                   18.692(8)
_cell_measurement_reflns_used    213
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.35
_cell_measurement_theta_min      2.17
_cell_volume                     911.0(7)
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    X-Seed
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1211
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9640
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.830
_diffrn_reflns_theta_max         24.830
_diffrn_reflns_theta_min         2.189
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6103
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 349 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.6(10)
_refine_ls_extinction_coef       0.013(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         1573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0642P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.635
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                1138
_reflns_number_total             1573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06054d2.cif
_cod_data_source_block           Water
_cod_database_code               7124986
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              82097
_shelx_hkl_checksum              17997