Anion and Cation Effects on Anion-Templated Assembly of Tetrahydroxytriptycene
White, Nicholas G.; MacLachlan, Mark J.; Crystal Growth & Design 15 (2015) 5629–; doi:10.1021/acs.cgd.5b01342

data_4516544
_publ_section_title
;
 Anion and Cation Effects on Anion-Templated Assembly of
 Tetrahydroxytriptycene
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5629
_journal_paper_doi               10.1021/acs.cgd.5b01342
_journal_volume                  15
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_compound_source        synthesized
_chemical_formula_moiety         '0.5 (C22 H18 O4), C12 H28 N, Br'
_chemical_formula_sum            'C23 H37 Br N O2'
_chemical_formula_weight         439.45
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 110.784(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.710(4)
_cell_length_b                   8.607(2)
_cell_length_c                   18.326(6)
_cell_measurement_reflns_used    4355
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.38
_cell_volume                     2316.7(11)
_computing_cell_refinement       'Apex2, (Bruker, 2007)'
_computing_data_collection       'Apex2, (Bruker, 2007)'
_computing_data_reduction        'Apex2, (Bruker, 2007)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10567
_diffrn_reflns_theta_full        26.326
_diffrn_reflns_theta_max         26.326
_diffrn_reflns_theta_min         2.377
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.791
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             931.993
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.99
_refine_ls_abs_structure_details 'Flack (1983), 2139 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.083(8)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4640
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.0008498
_refine_ls_shift/su_mean         0.0000313
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 4.80 6.68 3.25 0.878 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0763
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0763
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3901
_reflns_number_total             4661
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.72
_oxford_diffrn_Wilson_scale      49.82
_oxford_refine_ls_r_factor_ref   0.0397
_oxford_refine_ls_scale          0.14703(5)
_oxford_reflns_number_all        4640
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  83,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  51,X'S) H   ( 512,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 533,X'S) H   ( 531,X'S) 
RIDE C   (  61,X'S) H   ( 612,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 622,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 633,X'S) H   ( 632,X'S) 
RIDE C   (  71,X'S) H   ( 712,X'S) H   ( 711,X'S) 
RIDE C   (  72,X'S) H   ( 722,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 732,X'S) H   ( 731,X'S) H   ( 733,X'S) 
RIDE C   (  81,X'S) H   ( 812,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 822,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 833,X'S) H   ( 831,X'S) H   ( 832,X'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            cg5b01342_si_002.cif
_cod_data_source_block           TPA
_cod_original_sg_symbol_H-M      'C 1 2 1 '
_cod_original_formula_sum        'C23 H37.00 Br1 N1 O2'
_cod_database_code               4516544