Use of modulators and light to control crystallisation of a hydrogen bonded framework
Muang-Non, Phonlakrit; Toop, Hamish D.; Doonan, Christian J.; White, Nicholas G.; Chemical Communications  (2022) –; doi:10.1039/D1CC06164J

data_7129379
_publ_section_title
;
 Use of modulators and light to control crystallisation of a hydrogen
 bonded framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06164J
_journal_year                    2022
_chemical_formula_moiety         'C29 H32 N8, 2(C14 H8 N2 O4)'
_chemical_formula_sum            'C57 H48 N12 O8'
_chemical_formula_weight         1029.07
_chemical_properties_physical    'Rapidly loses solvent'
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2021-10-27 deposited with the CCDC.	2021-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.440(4)
_cell_length_b                   25.440(4)
_cell_length_c                   7.3400(15)
_cell_measurement_reflns_used    64383
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.367
_cell_measurement_theta_min      0.800
_cell_volume                     4750.4(14)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX2 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            64383
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         0.800
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_description       rod
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water/ethanol'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
TITL 35_sq_sq_sq_sq_sqP 42/n_sq    R = 0.05
CELL   25.4400   25.4400    7.3400     90.00     90.00     90.00
SPGR P42/n
C101 0.958 0.734 0.254 !       5.55 eA-3
C102 0.447 0.271 0.362 !       4.01 eA-3
C103 0.125 0.953 0.082 !       3.47 eA-3
C104 0.869 0.436 0.619 !       2.94 eA-3
C105 0.307 0.490 0.335 !       2.86 eA-3
C106 0.895 0.334 0.134 !       1.93 eA-3
C107 0.442 0.799 0.193 !       1.79 eA-3
C108 0.968 0.274 0.498 !       1.70 eA-3
C109 0.903 0.191 0.478 !       1.55 eA-3
C110 0.059 0.709 0.342 !       1.43 eA-3
Q111 0.368 0.526 0.257 !       1.41 eA-3
C112 0.639 0.409 0.027 !       1.36 eA-3
C113 0.332 0.755 0.737 !       1.20 eA-3
C114 0.835 0.258 0.359 !       1.17 eA-3
C115 0.623 0.392 0.467 !       1.11 eA-3
C116 0.443 0.712 0.161 !       1.10 eA-3
C117 0.979 0.253 0.323 !       1.06 eA-3
C118 0.689 0.268 0.124 !       1.05 eA-3
C119 0.359 0.779 0.072 !       0.89 eA-3
C120 0.198 0.712 0.409 !       0.88 eA-3
C121 0.586 0.297 0.843 !       0.87 eA-3
C122 0.132 0.647 0.157 !       0.86 eA-3
C123 0.391 0.718-0.003 !       0.85 eA-3
C124 0.789 0.196-0.010 !       0.83 eA-3
C125 0.646 0.263 0.535 !       0.78 eA-3
C126 0.890 0.214 0.620 !       0.75 eA-3
Q127 0.117 0.591 0.750 !       0.75 eA-3
C128 0.821 0.297 0.295 !       0.71 eA-3
C129 0.050 0.749 0.065 !       0.68 eA-3
C130 0.867 0.376 0.299 !       0.67 eA-3
C131 0.834 0.270 0.620 !       0.67 eA-3
C132 0.128 0.618 0.637 !       0.66 eA-3
C133 0.327 0.749 0.292 !       0.65 eA-3
C134 0.400 0.758 0.375 !       0.61 eA-3
Q135 0.858 0.985 0.086 !       0.57 eA-3
C136 0.954 0.228 0.153 !       0.57 eA-3
Q137 0.397 0.306 0.342 !       0.57 eA-3
C138 0.320 0.733 0.382 !       0.55 eA-3
C139 0.130 0.790 0.869 !       0.54 eA-3
C140 0.763 0.365 0.785 !       0.54 eA-3
Q141 0.820 1.000 0.087 !       0.54 eA-3
Q142 0.994 0.675 0.491 !       0.52 eA-3
C143 0.180 0.805 0.320 !       0.52 eA-3
C144 0.205 0.978 0.137 !       0.51 eA-3
C145 0.823 0.429 0.407 !       0.51 eA-3
Q146 0.328 0.951 0.067 !       0.50 eA-3
;
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4758
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1246P)^2^+0.8669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4717
_reflns_number_total             4758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06164j2.cif
_cod_data_source_block           1DiA2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'None' was changed
to 'none' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        4750.4(17)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7129379
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'