Anion templated crystal engineering of halogen bonding tripodal tris(halopyridinium) compounds
Foyle, Émer M.; White, Nicholas G.; CrystEngComm  (2020) –; doi:10.1039/D0CE00241K

data_7240175
_publ_section_title
;
 Anion templated crystal engineering of halogen bonding tripodal
 tris(halopyridinium) compounds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00241K
_journal_year                    2020
_chemical_formula_moiety         '3(I), C42 H57 Br3 N3 O3'
_chemical_formula_sum            'C42 H57 Br3 I3 N3 O3'
_chemical_formula_weight         1272.36
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2020-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.82(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.822(3)
_cell_length_b                   20.352(4)
_cell_length_c                   17.306(4)
_cell_measurement_reflns_used    34125
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.371
_cell_measurement_theta_min      1.795
_cell_volume                     4812(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.9902
_diffrn_measured_fraction_theta_max 0.9902
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44151
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    4.477
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2464.7362
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.4883
_refine_diff_density_min         -2.0231
_refine_diff_density_rms         0.1713
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             11.3429
_refine_ls_goodness_of_fit_ref   1.0291
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     490
_refine_ls_number_reflns         9760
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.0280
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+26.2230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -18
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -10
_reflns_number_gt                8342
_reflns_number_total             9760
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ce00241k2.cif
_cod_data_source_block           EMF-1_a
_cod_database_code               7240175
_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
 C32-C31 = C30-C31
 1.53 with sigma of 0.005
 C29-C31
 2.55 with sigma of 0.02
 C30-C32
 2.55 with sigma of 0.02
3. Restrained angles
 C30-C31-C32
 fixed at 109.5 with sigma of 0.02
 C29-C30-C31
 fixed at 109.5 with sigma of 0.02
4. Rigid bond restraints
 C30, C31, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.001
6.a Secondary CH2 refined with riding coordinates:
 C48(H48a,H48b), C33(H33a,H33b), C18(H18a,H18b), C27(H27a,H27b), C11(H11a,
 H11b), C42(H42a,H42b), C12(H12a,H12b), C43(H43a,H43b), C28(H28a,H28b),
 C13(H13a,H13b), C44(H44a,H44b), C29(H29a,H29b), C14(H14a,H14b), C45(H45a,H45b),
  C15(H15a,H15b), C30(H30a,H30b), C46(H46a,H46b), C31(H31a,H31b)
6.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C35(H35), C36(H36), C37(H37), C54(H54), C50(H50), C51(H51),
 C52(H52), C24(H24), C20(H20), C21(H21), C22(H22)
6.c Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C47(H47a,H47b,H47c), C32(H32a,H32b,H32c)
;
_olex2_submission_special_instructions 'No special instructions were received'