Solid-State Examination of Conformationally Diverse Sulfonamide Receptors Based on Bis(2-anilinoethynyl)pyridine, -Bipyridine, and -Thiophene.
Berryman, Orion B.; Johnson, 2nd, Charles A; Vonnegut, Chris L.; Fajardo, Kevin A.; Zakharov, Lev N.; Johnson, Darren W.; Haley, Michael M.; Crystal growth & design 15 (2015) 1502–1511; doi:10.1021/cg5018856

data_4512693
_publ_section_title
;
 Solid-State Examination of Conformationally Diverse Sulfonamide Receptors
 Based on Bis(2-anilinoethynyl)pyridine, -Bipyridine, and -Thiophene.
;
_journal_issue                   3
_journal_name_full               'Crystal growth &amp; design'
_journal_page_first              1502
_journal_page_last               1511
_journal_paper_doi               10.1021/cg5018856
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C41 H37 N5 O8 S2, 0.5(C H Cl3)'
_chemical_formula_sum            'C41.5 H37.5 Cl1.5 N5 O8 S2'
_chemical_formula_weight         851.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.226(4)
_cell_length_b                   20.765(3)
_cell_length_c                   31.191(4)
_cell_measurement_reflns_used    8432
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      54.36
_cell_measurement_theta_min      4.84
_cell_volume                     17634(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            99288
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.505
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.9352
_exptl_absorpt_correction_T_min  0.8762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7088
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         20858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1329P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2096
_refine_ls_wR_factor_ref         0.2351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12313
_reflns_number_total             20858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5018856_si_002.cif
_cod_data_source_block           ob100
_cod_depositor_comments
;Adding full bibliography for 4512691--4512698.cif.

 Adding full bibliography for 4512691--4512698.cif.
;
_cod_database_code               4512693
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.924
_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.a Ternary CH refined with riding coordinates:
 C1S(H1S)
2.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C10(H10A), C11(H11), C13(H13), C19(H19), C20(H20),
 C22(H22), C23(H23), C27(H27), C29(H29), C30(H30), C37(H37), C38(H38), C40(H40),
  C41(H41), C43(H43), C44(H44), C45(H45), C49(H49), C51(H51), C52(H52),
 C54(H54), C57(H57), C59(H59), C60(H60), C69(H69), C71(H71), C72(H72), C78(H78),
  C79(H79), C81(H81), C82(H82)
;