A three dimensional hydrogen bonded organic framework assembled through antielectrostatic hydrogen bonds.
Cullen, Duncan A.; Gardiner, Michael G.; White, Nicholas G.; Chemical communications (Cambridge, England) 55 (2019) 12020–12023; doi:10.1039/c9cc06707h

data_7125414
_publ_section_title
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 A three dimensional hydrogen bonded organic framework assembled through
 antielectrostatic hydrogen bonds.
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_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12020
_journal_page_last               12023
_journal_paper_doi               10.1039/c9cc06707h
_journal_volume                  55
_journal_year                    2019
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C29 H28 N8, 4(C H4 O)'
_chemical_formula_sum            'C33 H44 N8 O4'
_chemical_formula_weight         616.76
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2019-08-26 deposited with the CCDC.	2019-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.533300(16)
_cell_length_b                   14.533300(16)
_cell_length_c                   7.836020(13)
_cell_measurement_reflns_used    3773
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.4
_cell_measurement_theta_min      6.08
_cell_volume                     1655.099(4)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'CrysAlisPro, (Agilent, 2011'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_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      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Supernova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_unetI/netI     0.008
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8618
_diffrn_reflns_theta_full        72.327
_diffrn_reflns_theta_max         73.803
_diffrn_reflns_theta_min         4.302
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             660
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol, acetone, diethyl ether'
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1635
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.0003060
_refine_ls_shift/su_mean         0.0000326
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 1.18P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1348
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1348
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                1588
_reflns_number_total             1665
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.19
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.0511
_oxford_refine_ls_scale          9.0(6)
_oxford_reflns_number_all        1635
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT N    (     2 ,X'S,U'S)  UNTIL C    (   102 ) 
CONT H    (    12 ,X'S,U[ISO])  UNTIL H    (  1011 ) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) H   (1022,X'S) H   (1023,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM NO H  NO #H U MULT   DIST 
REM C-H 
REM >4           1.5    .96 DISORDER 
REM 1      1     1.2    .93 C C-H (ACETYLENE) 
REM 1      2     1.2    .93 C-C(H)-C 
REM 1      3     1.2    .98 (C)3-C-H 
REM 2      1     1.2    .93 C=C-H(2) 
REM 2      2     1.2    .97 (C)2-C-(H)2 
REM 3      1     1.5    .96 C-C-(H)3 
REM N-H 
REM >4           1.5    .89 DISORDER 
REM 1      1     1.2    .86 N-N/H 
REM 1      2     1.2    .86 (C)2-N-H 
REM 1      3     1.2    .89 (C)3-N-H 
REM 2      1     1.2    .86 C-N-(H)2 
REM 2      2     1.2    .89 (C)2-N-(H)2 
REM 3      1     1.2    .89 C-H-(H)3 
REM O-H 
REM 1      1     1.5    .82 O-H 
REM 
REM DIST      ESD = 0.02 
REM VIB       ESD = 0.002 
REM ANGLE     ESD = 2.0 
REM 
REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM 
REM            H1-N-R1 
DIST 0.86, 0.02 = 
CONT N ( 2) TO H(21) 
REST 0.041, 0.002 = H(21,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(3) TO N ( 2) TO H(21) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 1) TO H(12) 
CONT N ( 1) TO H(11) 
REST 0.047, 0.002 = H(12,U[ISO]) 
REST 0.047, 0.002 = H(11,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(3) TO N ( 1) TO H(12) 
CONT C(3) TO N ( 1) TO H(11) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 101) TO H(1011) 
REST 0.057, 0.002 = H(1011,U[ISO]) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            c9cc06707h2.cif
_cod_data_source_block           2
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1655.099(5)
_cod_original_sg_symbol_H-M      'P 42/n '
_cod_database_code               7125414
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)