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_7241807
_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         'C41 H44 N3 O11 Zn2.5, 0.75(C3 H7 N O)'
_chemical_formula_sum            'C43.25 H49.25 N3.75 O11.75 Zn2.5'
_chemical_formula_weight         973.04
_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   mixed
_audit_creation_date             2020-04-15
_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                 94.4980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.8995(2)
_cell_length_b                   21.0392(2)
_cell_length_c                   32.8802(3)
_cell_measurement_reflns_used    14543
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      76.932
_cell_measurement_theta_min      3.911
_cell_volume                     14413.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            50261
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.932
_diffrn_reflns_theta_min         3.911
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.897
_exptl_crystal_description       plate
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.79798
_refine_diff_density_max         1.773
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.000077(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         14543
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0662
_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^)+(0.1352P)^2^+31.5538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12581
_reflns_number_total             14543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01620a2.cif
_cod_data_source_block           6Zn
_cod_depositor_comments
'Adding full bibliography for 7241796--7241816.cif.'
_cod_original_formula_sum        'C43.25 H49.25 N3.75 O11.75 Zn2.50'
_cod_database_code               7241807
_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, All O(H,H) groups
2. Restrained distances
 O12-C42
 1.2 with sigma of 0.02
 H10A-O4_$5
 1.899 with sigma of 0.02
 H10B-O12
 1.671 with sigma of 0.02
3. Restrained planarity
 O13, N5, C45, C46, C47
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.001
5. Others
 Fixed Sof: O12(0.5) N4(0.5) C42(0.5) H42(0.5) C43(0.5) H43A(0.5) H43B(0.5)
 H43C(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) O13(0.25) N5(0.25) C45(0.25)
 H45(0.25) C46(0.25) H46A(0.25) H46B(0.25) H46C(0.25) C47(0.25) H47A(0.25)
 H47B(0.25) H47C(0.25)
6.a Rotating group:
 O10(H10A,H10B)
6.b Ternary CH refined with riding coordinates:
 N2(H2), C1(H1), C4(H4)
6.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C15(H15A,
 H15B), C23(H23A,H23B), C31(H31A,H31B)
6.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C17(H17), C18(H18), C20(H20), C21(H21),
 C25(H25), C26(H26), C28(H28), C29(H29), C33(H33), C34(H34), C36(H36), C37(H37),
  C39(H39), C42(H42), C45(H45)
6.e Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              55818
_shelx_fab_checksum              68700
_olex2_submission_special_instructions 'No special instructions were received'