Single-crystal-to-single-crystal transformation of the desolvation of a cyclotriveratrylene–acetonitrile inclusion complex via a gating mechanism with subsequent polymorphism
Payne, Richard M.; Oliver, Clive L.; CrystEngComm 18 (2016) 7965–; doi:10.1039/C6CE01078D

data_7226528
_publ_section_title
;
 Single-crystal-to-single-crystal transformation of the desolvation of a
 cyclotriveratrylene--acetonitrile inclusion complex via a gating
 mechanism with subsequent polymorphism
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              7965
_journal_paper_doi               10.1039/C6CE01078D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C27 H30 O6, 0.5(C2 H3 N)'
_chemical_formula_sum            'C28 H31.5 N0.5 O6'
_chemical_formula_weight         471.04
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-07 deposited with the CCDC.
2016-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7531(8)
_cell_length_b                   25.0061(11)
_cell_length_c                   10.5276(5)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.32
_cell_volume                     4935.6(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            112892
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.517
_diffrn_reflns_theta_min         1.357
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         13782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.8135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8543
_reflns_number_total             13782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01078d2.cif
_cod_data_source_block           rpctvindo2
_cod_depositor_comments
'Adding full bibliography for 7226528--7226529.cif.'
_cod_original_formula_sum        'C28 H31.50 N0.50 O6'
_cod_database_code               7226528
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9A(H9AA,H9AB), C27A(H27A,H27B), C18A(H18A,H18B), C27B(H27C,H27D), C18B(H18C,
 H18D), C9B(H9BA,H9BB)
2.b Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C15A(H15A), C3A(H3A), C21A(H21A), C24A(H24A), C12A(H12A),
 C24B(H24B), C6B(H6B), C15B(H15B), C21B(H21B), C3B(H3B), C12B(H12B)
2.c Idealised Me refined as rotating group:
 C17A(H17A,H17B,H17C), C26A(H26A,H26B,H26C), C7A(H7AA,H7AB,H7AC), C16A(H16A,
 H16B,H16C), C8A(H8AA,H8AB,H8AC), C25A(H25A,H25B,H25C), C17B(H17D,H17E,H17F),
 C16B(H16D,H16E,H16F), C7B(H7BA,H7BB,H7BC), C25B(H25D,H25E,H25F), C8B(H8BA,H8BB,
 H8BC), C26B(H26D,H26E,H26F), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              9260
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'