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_7124980
_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 H8 N2 O4'
_chemical_formula_weight         196.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 82.466(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.7242(12)
_cell_length_b                   12.369(3)
_cell_length_c                   13.831(3)
_cell_measurement_reflns_used    6579
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      2.2
_cell_volume                     801.2(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(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  0.1669
_diffrn_reflns_av_unetI/netI     0.1436
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6579
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        23.309
_diffrn_reflns_theta_max         23.309
_diffrn_reflns_theta_min         2.217
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5421
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       plate
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1154
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.1138
_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^)+(0.0446P)^2^+3.6472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                719
_reflns_number_total             1154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06054d2.cif
_cod_data_source_block           USA
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7124980
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              33419
_shelx_hkl_checksum              31707