Highly Connected Framework Materials from Flexible Tetra-Isophthalate Ligands
Chahine, Ali; Chaffee, Alan L.; Knowles, Gregory P.; Turner, David Roger; Batten, Stuart R.; CrystEngComm  (2022) –; doi:10.1039/D2CE00269H

data_7244699
_publ_section_title
;
 Highly Connected Framework Materials from Flexible Tetra-Isophthalate
 Ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00269H
_journal_year                    2022
_chemical_formula_moiety         '2(Cl), C38 H34 N2 O16, 4(H2 O)'
_chemical_formula_sum            'C38 H42 Cl2 N2 O20'
_chemical_formula_weight         917.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-11-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                109.77(3)
_cell_angle_beta                 100.53(3)
_cell_angle_gamma                96.70(3)
_cell_formula_units_Z            1
_cell_length_a                   6.8800(14)
_cell_length_b                   11.900(2)
_cell_length_c                   15.690(3)
_cell_measurement_reflns_used    4607
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.371
_cell_measurement_theta_min      1.853
_cell_volume                     1166.2(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46771
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.853
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   0.4346
_exptl_transmission_factor_min   0.3694
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4712
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.6189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4607
_reflns_number_total             4712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00269h2.cif
_cod_data_source_block           L1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' 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        1166.1(5)
_cod_database_code               7244699
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Cl1_$2-H9B
 2.25 with sigma of 0.02
3.a Free rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
3.b Ternary CH refined with riding coordinates:
 N1(H1A)
3.c Secondary CH2 refined with riding coordinates:
 C1(H1B,H1C), C2(H2A,H2B), C3(H3A,H3B)
3.d Aromatic/amide H refined with riding coordinates:
 C5(H5A), C7(H7A), C9(H9), C13(H13), C15(H15), C17(H17)
3.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3), O5(H5), O7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30094
_shelx_fab_checksum              68220
_olex2_submission_special_instructions 'No special instructions were received'