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_7241798
_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         'C46 H46 N2 O8, 8.5(H2 O), C3 H7 N O'
_chemical_formula_sum            'C49 H70 N3 O17.5'
_chemical_formula_weight         981.02
_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     dual
_audit_creation_date             2020-04-14
_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                85.640(2)
_cell_angle_beta                 75.452(2)
_cell_angle_gamma                86.886(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2759(2)
_cell_length_b                   11.7985(2)
_cell_length_c                   13.6442(3)
_cell_measurement_reflns_used    7805
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      75.0580
_cell_measurement_theta_min      3.7670
_cell_volume                     1284.96(5)
_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_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     37.00  68.00   0.50    0.26    --   47.70 -79.00 -60.00   62
  2  \w     45.00  92.00   0.50    0.26    --   47.70-125.00 -30.00   94
  3  \w     48.00  74.00   0.50    1.03    --  106.49 -79.00 -60.00   52
  4  \w     73.00 105.00   0.50    1.03    --  106.49 -94.00 -90.00   64
  5  \w     70.00 104.00   0.50    1.03    --  106.49 -94.00-180.00   68
  6  \w     34.00  66.00   0.50    1.03    --  106.49 -30.00 -90.00   64
  7  \w     36.00  64.00   0.50    1.03    --  106.49 -30.00-150.00   56
  8  \w     39.00  64.00   0.50    1.03    --  106.49 -30.00-180.00   50
  9  \w     33.00  64.00   0.50    1.03    --  106.49 -30.00-120.00   62
 10  \w     37.00  63.00   0.50    1.03    --  106.49 -30.00 -60.00   52
 11  \w     32.00  58.00   0.50    1.03    --  106.49 -30.00   0.00   52
 12  \w     33.00  66.00   0.50    1.03    --  106.49 -30.00  60.00   66
 13  \w     46.00  72.00   0.50    1.03    --  106.49 -45.00  90.00   52
 14  \w     33.00  58.00   0.50    1.03    --  106.49 -30.00 120.00   50
 15  \w     32.00  65.00   0.50    1.03    --  106.49 -30.00  90.00   66
 16  \w    105.00 178.00   0.50    1.03    --  106.49  30.00  30.00  146
 17  \w    102.00 178.00   0.50    1.03    --  106.49  30.00   0.00  152
 18  \w     83.00 162.00   0.50    1.03    --  106.49  79.00  63.00  158
 19  \w     62.00 117.00   0.50    0.26    --   47.70  79.00  63.00  110
 20  \w     44.00 104.00   0.50    1.03    --  106.49 -94.00 -30.00  120
 21  \w     68.00 105.00   0.50    1.03    --  106.49 -94.00  30.00   74
 22  \w     54.00 105.00   0.50    1.03    --  106.49 -94.00   0.00  102
 23  \w     35.00 103.00   0.50    1.03    --  106.49 -94.00 120.00  136
 24  \w     66.00  92.00   0.50    1.03    --  106.49 -94.00 150.00   52
 25  \w     34.00 105.00   0.50    1.03    --  106.49 -94.00  60.00  142
 26  \w     34.00  70.00   0.50    1.03    --  106.49 -94.00 -90.00   72
 27  \w     36.00  90.00   0.50    1.03    --  106.49 -94.00-150.00  108
 28  \w     35.00 101.00   0.50    1.03    --  106.49 -94.00-120.00  132
 29  \w    -51.00  11.00   0.50    0.26    --  -47.70  79.00  63.00  124
 30  \w    -60.00 -35.00   0.50    1.03    --  -86.25  79.00  63.00   50
 31  \w    -84.00 -23.00   0.50    0.26    --  -47.70 125.00 -30.00  122
 32  \w    -78.00 -51.00   0.50    1.03    --  -86.25  45.00-120.00   54
 33  \w   -121.00 -79.00   0.50    0.26    --  -47.70 -37.00 -30.00   84
 34  \w    -73.00 -42.00   0.50    0.26    --  -47.70 -37.00 -30.00   62
 35  \w   -108.00 -82.00   0.50    1.03    --  -86.25 -79.00 -60.00   52
 36  \w   -114.00 -27.00   0.50    0.26    --  -47.70 -79.00 -60.00  174
 37  \w   -118.00 -73.00   0.50    0.26    --  -47.70-125.00  30.00   90
 38  \w   -155.00-128.00   0.50    1.03    --  -86.25 -79.00 -60.00   54
 39  \w   -155.00-102.00   0.50    1.03    --  -86.25-125.00   0.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0457630000
_diffrn_orient_matrix_UB_12      0.0609901000
_diffrn_orient_matrix_UB_13      0.0997333000
_diffrn_orient_matrix_UB_21      0.1850540000
_diffrn_orient_matrix_UB_22      -0.0064004000
_diffrn_orient_matrix_UB_23      0.0031788000
_diffrn_orient_matrix_UB_31      0.0263808000
_diffrn_orient_matrix_UB_32      0.1158036000
_diffrn_orient_matrix_UB_33      -0.0608868000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.989
_diffrn_reflns_theta_min         3.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74357
_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    1.259
_exptl_crystal_description       plate
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.74357
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0003(9)
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0780
_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^)+(0.1499P)^2^+0.9329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2317
_refine_ls_wR_factor_ref         0.2445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4384
_reflns_number_total             5229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01620a2.cif
_cod_data_source_block           L2_DMF_H2O
_cod_depositor_comments
'Adding full bibliography for 7241796--7241816.cif.'
_cod_original_formula_sum        'C49 H70 N3 O17.50'
_cod_database_code               7241798
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C23 H23 N2 O8'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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) groups, All O(H,H) groups
2. Restrained distances
 O2_$1-H3
 1.69 with sigma of 0.04
 H9A-O7_$1
 1.699 with sigma of 0.02
 H9B-O10
 1.982 with sigma of 0.02
 O13-H9A
 1.929 with sigma of 0.01
 H13C-O1_$2
 1.86 with sigma of 0.01
 H13D-O5
 2.59 with sigma of 0.01
3. Others
 Fixed Sof: O5(0.5) N2(0.5) C24(0.5) H24(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C26(0.5) H26A(0.5) H26C(0.5) H26B(0.5) O13(0.5) H13C(0.5) H13D(0.5)
 O7(0.5) O8(0.5) H8B(0.5) H8A(0.5) O9(0.5) H9A(0.5) H9B(0.5) O10(0.5) O11(0.5)
 O12(0.25)
4.a Free rotating group:
 O6(H6A,H6B), O13(H13C,H13D), O8(H8B,H8A), O9(H9A,H9B)
4.b Ternary CH refined with riding coordinates:
 N1(H1), C11(H11)
4.c Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C5(H5), C6(H6), C8(H8), C9(H9), C16(H16), C17(H17), C19(H19),
  C20(H20), C21(H21), C22(H22), C24(H24)
4.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26C,H26B)
4.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              89122
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.960
_oxdiff_exptl_absorpt_empirical_full_min 0.574