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_7129380
_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(C16 H10 O4)'
_chemical_formula_sum            'C61 H52 N8 O8'
_chemical_formula_weight         1025.10
_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_creation_date             2021-08-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_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                   25.779(4)
_cell_length_b                   25.779(4)
_cell_length_c                   7.4300(15)
_cell_measurement_reflns_used    65639
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.790
_cell_volume                     4937.7(15)
_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 0.963
_diffrn_measured_fraction_theta_max 0.958
_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  0.0877
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            65639
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         0.790
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_description       rod
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water/ethanol'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
TITL 42_sq_sq_sq_sq_sqP 42/n       R = 0.06
CELL   25.7790   25.7790    7.4300     90.00     90.00     90.00
SPGR P42/n
C101 0.265 0.045 0.243 !       4.80 eA-3
C102 0.765 0.945 0.133 !       3.90 eA-3
C103 0.811 0.510 0.339 !       3.05 eA-3
Q104 0.053 0.649 0.154 !       2.90 eA-3
C105 0.826 0.097 0.004 !       1.43 eA-3
C106 0.039 0.862 0.373 !       1.39 eA-3
C107 0.816 0.279-0.001 !       1.11 eA-3
C108 0.055 0.844 0.517 !       1.03 eA-3
C109 0.721 0.305 0.391 !       1.01 eA-3
C110 0.957 0.202 0.081 !       0.93 eA-3
C111 0.118 0.879 0.879 !       0.93 eA-3
C112 0.658 0.102 0.341 !       0.92 eA-3
C113 0.446 0.784 0.806 !       0.87 eA-3
C114 0.299 0.945 0.198 !       0.84 eA-3
C115 0.407 0.798 0.903 !       0.80 eA-3
C116 0.243 0.654 0.859 !       0.79 eA-3
C117 0.510 0.271 0.492 !       0.75 eA-3
C118 0.680 0.225 0.669 !       0.73 eA-3
C119 0.893 0.283 0.030 !       0.73 eA-3
C120 0.733 0.061 0.783 !       0.72 eA-3
C121 0.738 0.172 0.245 !       0.72 eA-3
C122 0.086 0.831 0.044 !       0.72 eA-3
C123 0.207 0.659 0.217 !       0.68 eA-3
C124 0.244 0.539 0.470 !       0.67 eA-3
C125 0.356 0.710 0.885 !       0.65 eA-3
C126 0.645 0.280 0.174 !       0.64 eA-3
C127 0.711 0.203 0.371 !       0.64 eA-3
Q128 0.582 0.089 0.096 !       0.62 eA-3
Q129 0.616 0.414 0.742 !       0.60 eA-3
C130 0.329 0.788 0.558 !       0.59 eA-3
C131 0.298 0.838 0.836 !       0.57 eA-3
C132 0.740 0.306 0.007 !       0.56 eA-3
C133 0.647 0.374 0.746 !       0.56 eA-3
Q134 0.906 0.420 0.338 !       0.56 eA-3
C135 0.547 0.239 0.398 !       0.56 eA-3
Q136 0.093 0.557 0.783 !       0.56 eA-3
Q137 0.909 0.752 0.103 !       0.55 eA-3
C138 0.620 0.084 0.841 !       0.55 eA-3
C139 0.198 0.858 0.216 !       0.54 eA-3
;
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0647
_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^)+(0.1432P)^2^+0.2761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4745
_reflns_number_total             4846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06164j2.cif
_cod_data_source_block           1SB2
_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        4937.7(17)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7129380
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.569(2)
 0.431(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C5(H5), C6(H6), C8(H8),
 C9(H9)
3.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'