A linker conformation induced metal–organic framework with high stability and efficient upgrading of natural gas
Li, Shi-Ming; Jiang, Hong-Chan; Ni, Qing-Ling; Gui, Liu-Cheng; Wang, Xiu-Jian; Dalton Transactions  (2023) –; doi:10.1039/D3DT00979C

data_7713262
_publ_section_title
;
 A linker conformation induced metal--organic framework with high
 stability and efficient upgrading of natural gas
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00979C
_journal_year                    2023
_chemical_formula_moiety         'C26 H19 Cu3 N O15, 4[CH3CN], 2[H2O]'
_chemical_formula_sum            'C26 H19 Cu3 N O15'
_chemical_formula_weight         776.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-23 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7215(3)
_cell_length_b                   35.1471(8)
_cell_length_c                   19.2775(5)
_cell_measurement_reflns_used    8715
_cell_measurement_temperature    295.9(3)
_cell_measurement_theta_max      76.1180
_cell_measurement_theta_min      2.5070
_cell_volume                     9297.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (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  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -122.00 -42.00   0.50   14.26    --  -47.95 -23.00 -74.00  160
  2  \w   -120.00 -82.00   0.50   57.03    --  -86.25-116.00  83.00   76
  3  \w   -152.00-126.00   0.50   57.03    --  -86.25-116.00  83.00   52
  4  \w    106.00 162.00   0.50   57.03    --  107.75 105.00 -89.00  112
  5  \w    -20.00  20.00   0.50   14.26    --  -47.95  19.00 120.00   80
  6  \w    -23.00   9.00   0.50   14.26    --   47.95 -19.00-180.00   64
  7  \w    -42.00 -16.00   0.50   57.03    --  -86.25  37.00  90.00   52
  8  \w    -40.00 -15.00   0.50   57.03    --  -86.25  37.00 120.00   50
  9  \w     35.00  60.00   0.50   57.03    --  107.75 -57.00-120.00   50
 10  \w     35.00  61.00   0.50   57.03    --  107.75 -57.00-180.00   52
 11  \w     53.00  90.00   0.50   57.03    --  107.75 -99.00-180.00   74
 12  \w     43.00 106.00   0.50   57.03    --  107.75 -77.00  60.00  126
 13  \w    101.00 176.00   0.50   57.03    --  107.75  23.00  90.00  150
;
_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      0.0321255000
_diffrn_orient_matrix_UB_12      0.0317791000
_diffrn_orient_matrix_UB_13      0.0500924000
_diffrn_orient_matrix_UB_21      0.0051321000
_diffrn_orient_matrix_UB_22      0.0281789000
_diffrn_orient_matrix_UB_23      -0.0611320000
_diffrn_orient_matrix_UB_31      -0.1074004000
_diffrn_orient_matrix_UB_32      0.0108348000
_diffrn_orient_matrix_UB_33      0.0120004000
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14985
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        63.995
_diffrn_reflns_theta_max         63.995
_diffrn_reflns_theta_min         2.514
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.109
_exptl_crystal_description       needle
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4018
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2797
_refine_ls_wR_factor_ref         0.2931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3255
_reflns_number_total             4018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00979c2.cif
_cod_data_source_block           GNU-1
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7713262
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu'
_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 O(H,H) groups
2. Restrained distances
 O25-H25A = O25-H25B
 0.85 with sigma of 0.02
 O26-H26A = O26-H26B
 0.85 with sigma of 0.02
 O27-H27A = O27-H27B
 0.85 with sigma of 0.02
 H27A-H27B
 1.34 with sigma of 0.04
 H25A-H25B
 1.34 with sigma of 0.04
 H26A-H26B
 1.34 with sigma of 0.04
 Cu2-H27A \\sim Cu2-H27B
 with sigma of 0.02
 Cu3-H25A \\sim Cu3-H25B
 with sigma of 0.02
 Cu1-H26A \\sim Cu1-H26B
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C18(H18), C7(H7), C9(H9), C13(H13)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 877 electrons were 
found in a volume of 4957\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[CH3CN], 2[H2O] per Asymmetric Unit 
which account for 864 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.508
_oxdiff_exptl_absorpt_empirical_full_min 0.691