Structural diversity and solvent-induced transformations of a copper-based metal-organic framework with highly aromatic ligands.
Edwards, Abigail; Elkins, Landon J.; Slebodnick, Carla; Wang, Jinglei; Zhang, Qiang; Makal, Tegan A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14496–14504; doi:10.1039/d4dt02085e

data_7716813
_publ_section_title
;
 Structural diversity and solvent-induced transformations of a
 copper-based metal-organic framework with highly aromatic ligands.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14496
_journal_page_last               14504
_journal_paper_doi               10.1039/d4dt02085e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C52 H40 Cu2 N2 O10, 3[C4H9N1O1]'
_chemical_formula_sum            'C64 H67 Cu2 N5 O13'
_chemical_formula_weight         1241.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-11 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.982(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7147(2)
_cell_length_b                   37.1847(6)
_cell_length_c                   14.7691(2)
_cell_measurement_reflns_used    12078
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9760
_cell_measurement_theta_min      3.7750
_cell_volume                     5876.38(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_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    -83.00 -10.00   0.50    1.00    --  -45.04 119.00 122.00  146
  2  \w   -117.00 -60.00   0.50    1.00    --  -45.04-158.00-117.00  114
  3  \w     40.00  65.00   0.50    1.00    --   45.04-119.00  36.00   50
  4  \w     59.00  84.00   0.50    1.00    --   45.04-158.00-117.00   50
  5  \w   -142.00-117.00   0.50    5.00    --  -88.50-119.00  36.00   50
  6  \w   -121.00 -96.00   0.50    5.00    --  -88.50-158.00-117.00   50
  7  \w    -76.00 -51.00   0.50    5.00    --  -88.50 119.00 122.00   50
  8  \w    -93.00 -68.00   0.50    5.00    --  -88.50 158.00 -83.00   50
  9  \w     93.00 129.00   0.50    5.00    --  110.00-158.00-117.00   72
 10  \w     75.00 108.00   0.50    5.00    --  110.00-119.00  36.00   66
 11  \w    105.00 142.00   0.50    5.00    --  110.00 119.00 122.00   74
 12  \w     88.00 128.00   0.50    5.00    --  110.00 158.00 -83.00   80
 13  \w   -114.00 -85.00   0.50    1.00    --  -45.04 -77.00  90.00   58
 14  \w   -117.00 -88.00   0.50    1.00    --  -45.04 -77.00-150.00   58
 15  \w   -111.00 -86.00   0.50    1.00    --  -45.04 -77.00 -60.00   50
 16  \w   -118.00 -89.00   0.50    1.00    --  -45.04 -77.00  30.00   58
 17  \w   -113.00 -85.00   0.50    1.00    --  -45.04 -77.00 -30.00   56
 18  \w     92.00 118.00   0.50    1.00    --   45.04  77.00 -90.00   52
 19  \w    -67.00 -15.00   0.50    5.00    --  -88.50  61.00 -30.00  104
 20  \w    -48.00 -16.00   0.50    5.00    --  -88.50  45.00 -60.00   64
 21  \w    -51.00 -15.00   0.50    5.00    --  -88.50  45.00 -30.00   72
 22  \w     42.00  69.00   0.50    5.00    --  110.00 -61.00 -90.00   54
 23  \w     38.00 101.00   0.50    5.00    --  110.00 -94.00-150.00  126
 24  \w    114.00 173.00   0.50    5.00    --  110.00  30.00  90.00  118
 25  \w    132.00 178.00   0.50    5.00    --  110.00  30.00 120.00   92
 26  \w     97.00 173.00   0.50    5.00    --  110.00  45.00 -60.00  152
 27  \w     42.00  67.00   0.50    5.00    --  110.00 -61.00  90.00   50
 28  \w     40.00  92.00   0.50    5.00    --  110.00-125.00 -30.00  104
 29  \w     98.00 128.00   0.50    5.00    --  110.00  30.00 120.00   60
 30  \w     45.00 102.00   0.50    5.00    --  110.00 -94.00  90.00  114
 31  \w     61.00 105.00   0.50    5.00    --  110.00 -94.00   0.00   88
 32  \w     38.00 106.00   0.50    5.00    --  110.00 -94.00  30.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction XtaLAB Synergy, Dualflex, HyPix 6000-HE'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1097349000
_diffrn_orient_matrix_UB_12      0.0073307000
_diffrn_orient_matrix_UB_13      -0.0609151000
_diffrn_orient_matrix_UB_21      -0.0070250000
_diffrn_orient_matrix_UB_22      0.0404133000
_diffrn_orient_matrix_UB_23      0.0222805000
_diffrn_orient_matrix_UB_31      0.0929533000
_diffrn_orient_matrix_UB_32      -0.0055353000
_diffrn_orient_matrix_UB_33      0.0818057000
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            47605
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         74.503
_diffrn_reflns_theta_min         3.223
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.71a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         11844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0770P)^2^+3.5511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9193
_reflns_number_total             11844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02085e2.cif
_cod_data_source_block           cs2945
_cod_depositor_comments
'Adding full bibliography for 7716813--7716817.cif.'
_cod_database_code               7716813
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C61 H62 Cu2 N4 O13'
_chemical_oxdiff_usercomment     'Trevor Makal - UVA Wise  (TM3125-08)'
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C18(H18), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C40(H40), C42(H42)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 558 electrons were 
found in a volume of 1996\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C4H9N1O1] per asymmetric Unit 
which account for 576 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45445
_shelx_fab_checksum              15588
_olex2_date_sample_data_collection 2022-11-03
_olex2_date_sample_submission    2022-11-03
_olex2_submission_original_sample_id TM3125-08
_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 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.726