A diamondoid net sustained by halogen bonds: employing a cyclobutane to generate a tetrahedral architecture
Oburn, Shalisa M.; Santana, Carlos; Elacqua, Elizabeth; Groeneman , Ryan; CrystEngComm  (2020) –; doi:10.1039/D0CE00627K

data_7240540
_publ_section_title
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 A diamondoid net sustained by halogen bonds: employing a cyclobutane to
 generate a tetrahedral architecture
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00627K
_journal_year                    2020
_chemical_formula_moiety         '2(C6 Cl4 I2), C24 H20 N4, 2(C7 H8)'
_chemical_formula_sum            'C50 H36 Cl8 I4 N4'
_chemical_formula_weight         1484.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-04-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-20 deposited with the CCDC.	2020-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0411(4)
_cell_length_b                   16.8624(7)
_cell_length_c                   28.2059(7)
_cell_measurement_reflns_used    9616
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.32
_cell_volume                     5251.4(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            55382
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.287
_diffrn_reflns_theta_min         2.320
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 3067 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6505
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+5.3941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0319
_refine_ls_wR_factor_ref         0.0323
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6413
_reflns_number_total             6505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00627k2.cif
_cod_data_source_block           g23719
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7240540
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C5A \\sim C4A \\sim C3A \\sim C2A \\sim C6A \\sim C1A \\sim C7A: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C4A) = Uanis(C5A) = Uanis(C6A) = Uanis(C1A) = Uanis(C2A) = Uanis(C3A)
3. Rigid body (RIGU) restrains
 C6B, C3B, C2B, C7B, C1B, C4B, C5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6A, C5A, C4A, C3A, C2A, C1A, C7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C2A(0.5) H2A(0.5) C1A(0.5) C6A(0.5) H6A(0.5) C5A(0.5) H5A(0.5)
 C4A(0.5) H4A(0.5) C3A(0.5) H3A(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5)
 C1B(0.5) H1B(0.5) C2B(0.5) C3B(0.5) H3B(0.5) C6B(0.5) H6B(0.5) C5B(0.5)
 H5B(0.5) C4B(0.5) H4B(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C6(H6)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C5(H5), C4(H4), C11(H11), C7(H7), C8(H8), C2(H2), C1(H1), C2A(H2A),
 C6A(H6A), C5A(H5A), C4A(H4A), C3A(H3A), C1B(H1B), C3B(H3B), C6B(H6B), C5B(H5B),
  C4B(H4B)
5.c Fitted hexagon refined as free rotating group:
 C2A(C1A,C6A,C5A,C4A,C3A), C1B(C2B,C3B,C6B,C5B,C4B)
5.d Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_shelx_res_checksum              66332
_olex2_submission_special_instructions 'No special instructions were received'