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_7244701
_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         'Cl, C39 H35 N2 O16, 3(H2 O)'
_chemical_formula_sum            'C39 H41 Cl N2 O19'
_chemical_formula_weight         877.19
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                83.42(3)
_cell_angle_beta                 80.88(3)
_cell_angle_gamma                78.36(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4300(19)
_cell_length_b                   9.790(2)
_cell_length_c                   21.430(4)
_cell_measurement_reflns_used    47129
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      0.966
_cell_volume                     1906.2(7)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_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_source         'MX2 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47129
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_min         0.966
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       plate
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   0.4376
_exptl_transmission_factor_min   0.3176
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0628
_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^)+(0.1417P)^2^+0.7186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1855
_refine_ls_wR_factor_ref         0.2104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6860
_reflns_number_total             7993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00269h2.cif
_cod_data_source_block           L2
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__diffrn_radiation_type' was replaced with
'_diffrn_radiation_type'.

Automatic conversion script
Id: cif_correct_tags 7550 2019-12-06 10:49:48Z antanas 

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_database_code               7244701
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H8 of O8, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups, H14 of O14, H12 of O12, H10 of O10, H15 of O15, H5 of O5,
   H2 of O2, H3 of O3
2.a Free rotating group:
 O17(H17A,H17B), O18(H18A,H18B), O19(H19C,H19D)
2.b Ternary CH refined with riding coordinates:
 N1(H1)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C31(H31A,H31B)
2.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C6(H6), C8(H8A), C12(H12A), C15(H15A), C18(H18), C24(H24), C27(H27),
 C30(H30), C33(H33), C36(H36), C39(H39)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3), O5(H5), O8(H8), O10(H10), O12(H12), O14(H14), O15(H15)
;
_shelx_res_checksum              60592
_olex2_submission_special_instructions 'No special instructions were received'