Soluble Tetraaminotriptycene Precursors.
White, Nicholas G.; MacLachlan, Mark J.; The Journal of organic chemistry 80 (2015) 8390–8397; doi:10.1021/acs.joc.5b01221

data_4036251
_publ_section_title
;
 Soluble Tetraaminotriptycene Precursors.
;
_journal_issue                   16
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8390
_journal_page_last               8397
_journal_paper_doi               10.1021/acs.joc.5b01221
_journal_volume                  80
_journal_year                    2015
_chemical_compound_source        synthesized
_chemical_formula_moiety
'C38 H26 N6 O2, C4 H10 O, 0.85(C H4 O), 1.15(H2 O)'
_chemical_formula_sum            'C42.85 H41.7 N6 O5'
_chemical_formula_weight         720.74
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 97.859(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.439(6)
_cell_length_b                   16.616(6)
_cell_length_c                   15.497(6)
_cell_measurement_reflns_used    6941
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.41
_cell_volume                     3683(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.989
_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  0.066
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29325
_diffrn_reflns_theta_full        27.131
_diffrn_reflns_theta_max         27.684
_diffrn_reflns_theta_min         1.806
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9585
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         5654
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.0004432
_refine_ls_shift/su_mean         0.0000335
_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: 
 9.29 13.8 6.45 1.58 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1917
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1917
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                3911
_reflns_number_total             8529
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.72
_oxford_diffrn_Wilson_scale      61.57
_oxford_refine_ls_r_factor_ref   0.1001
_oxford_refine_ls_scale          0.13050(10)
_oxford_reflns_number_all        5654
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            jo5b01221_si_002.cif
_cod_data_source_block           11
_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_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C42.85 H41.70 N6 O5'
_cod_database_code               4036251
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE N   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE N   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 383,X'S) H   ( 382,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 462,X'S) H   ( 461,X'S) H   ( 463,X'S) 
RIDE C   ( 101,X'S) H   (1013,X'S) H   (1011,X'S) H   (1012,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) H   (1022,X'S) 
RIDE C   ( 104,X'S) H   (1042,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1052,X'S) H   (1053,X'S) H   (1051,X'S) 
RIDE O   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1122,X'S) H   (1123,X'S) 
RIDE O   ( 121,X'S) H   (1212,X'S) H   (1211,X'S) 
RIDE O   ( 131,X'S) H   (1311,X'S) H   (1312,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
DIST 1.50, 0.005 = C(101) TO C(102), C(104) TO C(105) 
DIST 1.43, 0.005 = C(102) TO O(103), O(103) TO C(104) 
PLANAR C(101) C(102) O(103) C(104) C(105) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00100 = C(101) TO C(102) 
VIBR .0, 0.00100 = C(102) TO O(103) 
VIBR .0, 0.00200 = O(103) TO C(101) 
VIBR .0, 0.00100 = O(103) TO C(104) 
VIBR .0, 0.00200 = C(104) TO C(102) 
VIBR .0, 0.00100 = C(104) TO C(105) 
VIBR .0, 0.00200 = C(105) TO O(103) 
VIBR .0, 0.00100 = O(111) TO C(112) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.02000 = C(101) TO C(102) 
U(IJ) .0, 0.01000 = C(102) TO O(103) 
U(IJ) .0, 0.01000 = O(103) TO C(104) 
U(IJ) .0, 0.02000 = C(104) TO C(105) 
U(IJ) .0, 0.02000 = O(111) TO C(112) 
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                                                                             
;