Crystal engineering of coordination polymers using flexible tetracarboxylate linkers with embedded cyclohexyldiamine cores
Chahine, Ali Y.; Turner, David R.; Batten, Stuart R.; CrystEngComm 23 (2021) 569–590; doi:10.1039/D0CE01620A

data_7241797
_publ_section_title
;
 Crystal engineering of coordination polymers using flexible
 tetracarboxylate linkers with embedded cyclohexyldiamine cores
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              569
_journal_page_last               590
_journal_paper_doi               10.1039/D0CE01620A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C66 H64 N2 O8, 2(C4 H9 N O)'
_chemical_formula_sum            'C74 H82 N4 O10'
_chemical_formula_weight         1187.43
_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   geom
_audit_creation_date             2020-04-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-11-06 deposited with the CCDC.	2020-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                112.89(3)
_cell_angle_beta                 91.22(3)
_cell_angle_gamma                93.74(3)
_cell_formula_units_Z            1
_cell_length_a                   6.3000(13)
_cell_length_b                   15.210(3)
_cell_length_c                   17.390(4)
_cell_measurement_reflns_used    6056
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      1.273
_cell_volume                     1529.9(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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Dectris Eiger2 9M'
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29115
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.273
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.5498
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6056
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.1015
_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^)+(0.1367P)^2^+1.5412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2749
_refine_ls_wR_factor_ref         0.2934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4759
_reflns_number_total             6056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01620a2.cif
_cod_data_source_block           Me4L3
_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 

 Adding full bibliography for 7241796--7241816.cif.
;
_cod_original_cell_volume        1529.9(6)
_cod_database_code               7241797
_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 C(H,H,H) groups
2. Restrained distances
 O3A-C32
 1.32 with sigma of 0.02
 O3B-C32 = O4B-C32
 1.32 with sigma of 0.02
 O3A-O4A
 2.2 with sigma of 0.02
3. Others
 Fixed Sof: O3A(0.5) O4A(0.5) C21A(0.5) H21A(0.5) C22A(0.5) H22A(0.5)
 C27A(0.5) H27A(0.5) C28A(0.5) H28A(0.5) C30A(0.5) H30A(0.5) C31A(0.5)
 H31A(0.5) C33A(0.5) H33A(0.5) H33B(0.5) H33C(0.5) O3B(0.5) O4B(0.5) C21B(0.5)
 H21B(0.5) C22B(0.5) H22B(0.5) C27B(0.5) H27B(0.5) C28B(0.5) H28B(0.5)
 C30B(0.5) H30B(0.5) C31B(0.5) H31B(0.5) C33B(0.5) H33D(0.5) H33E(0.5)
 H33F(0.5) O5A(0.5) N2A(0.5) C34A(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C35A(0.5)
 C36A(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C37A(0.5) H37A(0.5) H37B(0.5)
 H37C(0.5) O5B(0.5) N2B(0.5) C34B(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C35B(0.5)
 C36B(0.5) H36D(0.5) H36E(0.5) H36F(0.5) C37B(0.5) H37D(0.5) H37E(0.5) H37F(0.5)
4.a Ternary CH refined with riding coordinates:
 N1(H1), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C24(H24), C25(H25), C21A(H21A), C22A(H22A), C27A(H27A), C28A(H28A), C30A(H30A),
  C31A(H31A), C21B(H21B), C22B(H22B), C27B(H27B), C28B(H28B), C30B(H30B),
 C31B(H31B)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C33A(H33A,H33B,H33C), C33B(H33D,H33E,H33F), C34A(H34A,H34B,
 H34C), C36A(H36A,H36B,H36C), C37A(H37A,H37B,H37C), C34B(H34D,H34E,H34F),
 C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F)
;
_shelx_res_checksum              67238
_olex2_submission_special_instructions 'No special instructions were received'