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_7241814
_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         'C42.5 H44.5 Co K2 N3.5 O9.5'
_chemical_formula_sum            'C42.5 H44.5 Co K2 N3.5 O9.5'
_chemical_formula_weight         893.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-19
_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                90
_cell_angle_beta                 100.76(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.349(7)
_cell_length_b                   12.005(2)
_cell_length_c                   26.750(5)
_cell_measurement_reflns_used    14245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.208
_cell_measurement_theta_min      1.550
_cell_volume                     10206(4)
_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 0.960
_diffrn_measured_fraction_theta_max 0.790
_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  0.0904
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.790
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            87115
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.790
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.208
_diffrn_reflns_theta_min         1.550
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       plate
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.4346
_exptl_transmission_factor_min   0.2728
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         14245
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.1093
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3293
_refine_ls_wR_factor_ref         0.3634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8114
_reflns_number_total             14245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01620a2.cif
_cod_data_source_block           14
_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_formula_sum        'C42.50 H44.50 Co K2 N3.50 O9.50'
_cod_database_code               7241814
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4B-C39B
 1.25 with sigma of 0.02
 N4B-C41B
 1.3 with sigma of 0.02
 O10B-C39B
 1.2 with sigma of 0.02
 N3-C42A
 1.5 with sigma of 0.02
 N4B-C40A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O9(0.5) N3(0.5) C40A(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C42(0.5)
 H42(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) O10B(0.5) N4B(0.5) C39B(0.5)
 H39B(0.5) C41B(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42A(0.25) H42A(0.25)
 H42B(0.25) H42C(0.25) O10A(0.5) N4A(0.5) C39A(0.5) H39A(0.5) C41A(0.5)
 H41D(0.5) H41E(0.5) H41F(0.5) C42B(0.25) H42D(0.25) H42F(0.25) H42E(0.25)
 C40B(0.5) H40D(0.5) H40E(0.5) H40F(0.5)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C23(H23A,H23B), C31(H31A,H31B)
5.c Me refined with riding coordinates:
 C42A(H42A,H42B,H42C), C42B(H42D,H42F,H42E)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C17(H17), C18(H18), C20(H20), C21(H21),
 C25(H25), C26(H26), C28(H28), C29(H29), C33(H33), C34(H34), C36(H36), C37(H37),
  C42(H42), C39B(H39B), C39A(H39A)
5.e Idealised Me refined as rotating group:
 C40A(H40A,H40B,H40C), C43(H43A,H43B,H43C), C41B(H41A,H41B,H41C), C41A(H41D,
 H41E,H41F), C40B(H40D,H40E,H40F)
;
_shelx_res_checksum              14356
_shelx_fab_checksum              46001
_olex2_submission_special_instructions 'No special instructions were received'