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_7124983
_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            'C11 H14 N2 O5'
_chemical_formula_weight         254.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 99.324(2)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   14.6759(9)
_cell_length_b                   31.2850(19)
_cell_length_c                   15.9269(10)
_cell_measurement_reflns_used    132
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.93
_cell_measurement_theta_min      2.42
_cell_volume                     7216.0(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_computing_molecular_graphics    XSeed
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            63443
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.070
_diffrn_reflns_theta_max         22.070
_diffrn_reflns_theta_min         2.061
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       rod
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.078
_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     985
_refine_ls_number_reflns         8899
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0790
_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^)+(0.0922P)^2^+19.1814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5728
_reflns_number_total             8899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06054d2.cif
_cod_data_source_block           Acetone
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7124983
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              18054
_shelx_hkl_checksum              41816