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_4516542
_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_compound_source        synthesized
_chemical_formula_moiety         'C22 H18 O4, C8 H20 N, 1.5(Br)'
_chemical_formula_sum            'C30 H38 Br1.5 N O4'
_chemical_formula_weight         596.49
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3023(19)
_cell_length_b                   35.513(4)
_cell_length_c                   12.0386(15)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      2.23
_cell_volume                     6542.1(14)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.043
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            35272
_diffrn_reflns_theta_full        25.796
_diffrn_reflns_theta_max         26.322
_diffrn_reflns_theta_min         1.786
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2476
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         2.08
_refine_diff_density_min         -1.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9539
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     156
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.0005505
_refine_ls_shift/su_mean         0.0000236
_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: 
 4.50 5.59 1.47 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2040
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2040
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              44
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                4627
_reflns_number_total             6717
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.27
_oxford_diffrn_Wilson_scale      399.78
_oxford_refine_ls_r_factor_ref   0.1054
_oxford_refine_ls_scale          0.060751(19)
_oxford_reflns_number_all        5478
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            cg5b01342_si_002.cif
_cod_data_source_block           TEAsqueeze
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        6542.2(14)
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C30 H38 Br1.50 N1 O4'
_cod_database_code               4516542
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,X'S) H   ( 203,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) H   ( 223,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) H   ( 523,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) H   ( 612,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 623,X'S) H   ( 622,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) H   ( 723,X'S) 
RIDE C   (  81,X'S) H   ( 812,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) H   ( 823,X'S) H   ( 822,X'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE O   (   7,X'S) H   (  71,X'S) 
RIDE O   (   8,X'S) H   (  81,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) H   (1512,X'S) 
RIDE C   ( 152,X'S) H   (1521,X'S) H   (1522,X'S) H   (1523,X'S) 
RIDE C   ( 161,X'S) H   (1611,X'S) H   (1612,X'S) 
RIDE C   ( 162,X'S) H   (1621,X'S) H   (1623,X'S) H   (1622,X'S) 
RIDE C   ( 171,X'S) H   (1711,X'S) H   (1712,X'S) 
RIDE C   ( 172,X'S) H   (1721,X'S) H   (1723,X'S) H   (1722,X'S) 
RIDE C   ( 181,X'S) H   (1812,X'S) H   (1811,X'S) 
RIDE C   ( 182,X'S) H   (1821,X'S) H   (1823,X'S) H   (1822,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
DIST 0, 0.005 = MEAN N(50) TO C(51), N(50) TO C(61) 
CONT N(50) TO C(71), N(50) TO C(81) 
CONT N(50) TO C(151), N(50) TO C(161) 
CONT N(50) TO C(171), N(50) TO C(181) 
DIST 0, 0.005 = MEAN C(51) TO C(52), C(61) TO C(62) 
CONT C(71) TO C(72), C(81) TO C(82) 
CONT C(151) TO C(152), C(161) TO C(162) 
CONT C(171) TO C(172), C(181) TO C(182) 
ANGL 0, 1 = MEAN N(50) TO C(51) TO C(52) 
CONT N(50) TO C(61) TO C(62) 
CONT N(50) TO C(71) TO C(72) 
CONT N(50) TO C(81) TO C(82) 
CONT N(50) TO C(151) TO C(152) 
CONT N(50) TO C(161) TO C(162) 
CONT N(50) TO C(171) TO C(172) 
CONT N(50) TO C(181) TO C(182) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00100 = N(50) TO C(51) 
VIBR .0, 0.00100 = N(50) TO C(61) 
VIBR .0, 0.00100 = N(50) TO C(71) 
VIBR .0, 0.00100 = N(50) TO C(81) 
VIBR .0, 0.00200 = C(61) TO C(51) 
VIBR .0, 0.00200 = C(71) TO C(51) 
VIBR .0, 0.00200 = C(71) TO C(61) 
VIBR .0, 0.00200 = C(81) TO C(51) 
VIBR .0, 0.00200 = C(81) TO C(61) 
VIBR .0, 0.00200 = C(81) TO C(71) 
VIBR .0, 0.00100 = C(51) TO C(52) 
VIBR .0, 0.00200 = C(52) TO N(50) 
VIBR .0, 0.00100 = C(61) TO C(62) 
VIBR .0, 0.00200 = C(62) TO N(50) 
VIBR .0, 0.00100 = C(71) TO C(72) 
VIBR .0, 0.00200 = C(72) TO N(50) 
VIBR .0, 0.00100 = C(81) TO C(82) 
VIBR .0, 0.00200 = C(82) TO N(50) 
VIBR .0, 0.00100 = N(50) TO C(151) 
VIBR .0, 0.00100 = N(50) TO C(161) 
VIBR .0, 0.00100 = N(50) TO C(171) 
VIBR .0, 0.00100 = N(50) TO C(181) 
VIBR .0, 0.00200 = C(161) TO C(151) 
VIBR .0, 0.00200 = C(171) TO C(151) 
VIBR .0, 0.00200 = C(171) TO C(161) 
VIBR .0, 0.00200 = C(181) TO C(151) 
VIBR .0, 0.00200 = C(181) TO C(161) 
VIBR .0, 0.00200 = C(181) TO C(171) 
VIBR .0, 0.00100 = C(151) TO C(152) 
VIBR .0, 0.00200 = C(152) TO N(50) 
VIBR .0, 0.00100 = C(161) TO C(162) 
VIBR .0, 0.00200 = C(162) TO N(50) 
VIBR .0, 0.00100 = C(171) TO C(172) 
VIBR .0, 0.00200 = C(172) TO N(50) 
VIBR .0, 0.00100 = C(181) TO C(182) 
VIBR .0, 0.00200 = C(182) TO N(50) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.01000 = N(50) TO C(51) 
U(IJ) .0, 0.01000 = N(50) TO C(61) 
U(IJ) .0, 0.01000 = N(50) TO C(71) 
U(IJ) .0, 0.01000 = N(50) TO C(81) 
U(IJ) .0, 0.01000 = N(50) TO C(151) 
U(IJ) .0, 0.01000 = N(50) TO C(161) 
U(IJ) .0, 0.01000 = N(50) TO C(171) 
U(IJ) .0, 0.01000 = N(50) TO C(181) 
U(IJ) .0, 0.02000 = C(51) TO C(52) 
U(IJ) .0, 0.02000 = C(61) TO C(62) 
U(IJ) .0, 0.02000 = C(71) TO C(72) 
U(IJ) .0, 0.02000 = C(81) TO C(82) 
U(IJ) .0, 0.02000 = C(151) TO C(152) 
U(IJ) .0, 0.02000 = C(161) TO C(162) 
U(IJ) .0, 0.02000 = C(171) TO C(172) 
U(IJ) .0, 0.02000 = C(181) TO C(182) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;