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_4516546
_publ_section_title
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 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 H4 O4, 2(C16 H36 N), C2 H3 N'
_chemical_formula_sum            'C64 H97 N3 O8'
_chemical_formula_weight         1036.45
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 101.570(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.696(2)
_cell_length_b                   31.604(8)
_cell_length_c                   9.801(2)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    90
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      4.61
_cell_volume                     2942.3(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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            29032
_diffrn_reflns_theta_full        63.406
_diffrn_reflns_theta_max         66.743
_diffrn_reflns_theta_min         4.605
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5178
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.0052014
_refine_ls_shift/su_mean         0.0000554
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 1.26P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1136
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1127
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              37
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                5032
_reflns_number_total             5230
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      64.60
_oxford_refine_ls_r_factor_ref   0.0438
_oxford_refine_ls_scale          0.12179(5)
_oxford_reflns_number_all        5202
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_iucr_refine_instructions_details_constraints
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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   (  92,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,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   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) H   ( 543,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   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) 
RIDE C   (  64,X'S) H   ( 642,X'S) H   ( 641,X'S) H   ( 643,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) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) 
RIDE C   (  74,X'S) H   ( 742,X'S) H   ( 741,X'S) H   ( 743,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) H   ( 812,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) H   ( 822,X'S) 
RIDE C   (  83,X'S) H   ( 832,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 843,X'S) H   ( 841,X'S) H   ( 842,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 203,X'S) H   (2032,X'S) H   (2031,X'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   4,X'S) H   (  41,X'S) 
RIDE C   (  94,X'S) H   ( 942,X'S) H   ( 941,X'S) H   ( 943,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) H   ( 932,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) H   ( 922,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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DIST 1.53, 0.01 = C(81) TO C(82) 
CONT C(82) TO C(83), C(83) TO C(84) 
CONT C(81) TO C(92), C(92) TO C(93) 
CONT C(93) TO C(94) 
ANGL 109, 1 = N(50) TO C(81) TO C(82) 
CONT C(81) TO C(82) TO C(83) 
CONT C(82) TO C(83) TO C(84) 
CONT C(81) TO C(92) TO C(93) 
CONT C(92) TO C(93) TO C(94) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = N(50) TO C(81) 
VIBR .0, 0.00500 = C(81) TO C(51) 
VIBR .0, 0.00500 = C(81) TO C(61) 
VIBR .0, 0.00500 = C(81) TO C(71) 
VIBR .0, 0.00200 = C(81) TO C(82) 
VIBR .0, 0.00500 = C(82) TO N(50) 
VIBR .0, 0.00200 = C(82) TO C(83) 
VIBR .0, 0.00500 = C(83) TO C(81) 
VIBR .0, 0.00200 = C(83) TO C(84) 
VIBR .0, 0.00500 = C(84) TO C(82) 
VIBR .0, 0.00200 = C(94) TO C(93) 
VIBR .0, 0.00200 = C(93) TO C(92) 
VIBR .0, 0.00500 = C(92) TO C(94) 
VIBR .0, 0.00500 = C(93) TO C(81) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = N(50) TO C(81) 
U(IJ) .0, 0.01000 = C(81) TO C(82) 
U(IJ) .0, 0.01000 = C(82) TO C(83) 
U(IJ) .0, 0.01000 = C(83) TO C(84) 
U(IJ) .0, 0.01000 = C(81) TO C(92) 
U(IJ) .0, 0.01000 = C(92) TO C(93) 
U(IJ) .0, 0.01000 = C(93) TO C(94) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
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           zigzagACP
_cod_depositor_comments
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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 
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_cod_original_cell_volume        2942.5(12)
_cod_original_sg_symbol_H-M      'P 21/m '
_cod_database_code               4516546