Structural variation determined by length-matching effects: towards the formation of flexible porous molecular crystals
Kai, Aiting; Sheng, Yujie; Yao, Junyao; Chen, Qibin; Liu, Honglai; CrystEngComm 20 (2018) 2648–; doi:10.1039/C7CE02245J

data_7230419
_publ_section_title
;
 Structural variation determined by length-matching effects: towards the
 formation of flexible porous molecular crystals
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              2648
_journal_paper_doi               10.1039/C7CE02245J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C34 H58 N2, 2(Br)'
_chemical_formula_sum            'C34 H58 Br2 N2'
_chemical_formula_weight         654.64
_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             2015-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2017-12-28 deposited with the CCDC.
2018-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.0410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0704(3)
_cell_length_b                   8.53580(10)
_cell_length_c                   17.9826(3)
_cell_measurement_reflns_used    2515
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      68.50
_cell_measurement_theta_min      5.12
_cell_volume                     1780.62(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9399
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.418
_diffrn_reflns_theta_min         5.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.4242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1207 before and 0.0524 after correction.
The Ratio of minimum to maximum transmission is 0.5632.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1090P)^2^+2.3161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2674
_reflns_number_total             3249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02245j2.cif
_cod_data_source_block           8-2Ar
_cod_depositor_comments
'Adding full bibliography for 7230419--7230420.cif.'
_cod_database_code               7230419
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.582
_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. Restrained distances
 C14-C13 = C16-C15 = C15-C14 = C17-C16
 1.52 with sigma of 0.01
 C13-C15 \\sim C14-C16
 with sigma of 0.02
 C15-C17 \\sim C14-C16
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              11119
_olex2_submission_special_instructions 'No special instructions were received'