Construction of Cu-based MOFs with enhanced hydrogenation performance by integrating open electropositive metal sites
Zhang, Xiuling; Geng, Longlong; Zhang, Yong-Zheng; Zhang, Da-Shuai; Zhang, Ranhui; Fu, Junna; Gao, Jun; Carozza, Jesse C.; Zhou, Zheng; Han, Haixiang; CrystEngComm 21 (2019) 5382–; doi:10.1039/C9CE01136F

data_7233407
_publ_section_title
;
 Construction of Cu-based MOFs with enhanced hydrogenation performance by
 integrating open electropositive metal sites
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5382
_journal_paper_doi               10.1039/C9CE01136F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C34 H28 Cu2 N4 O14'
_chemical_formula_sum            'C34 H28 Cu2 N4 O14'
_chemical_formula_weight         843.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-28 deposited with the CCDC.    2019-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2198(2)
_cell_length_b                   10.56080(10)
_cell_length_c                   21.3159(2)
_cell_measurement_reflns_used    5610
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.4520
_cell_measurement_theta_min      4.1510
_cell_volume                     3651.29(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11489
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.041
_diffrn_reflns_theta_max         67.041
_diffrn_reflns_theta_min         4.148
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3230
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0506
_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^)+(0.1010P)^2^+3.9343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2926
_reflns_number_total             3230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01136f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7233406--7233407.cif.'
_cod_database_code               7233407
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.789
_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. Uiso/Uaniso restraints and constraints
O5 \\sim N2 \\sim C15 \\sim C16 \\sim C17 \\sim O5X \\sim N2X \\sim C15X \\sim
C16X \\sim C17X: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Rigid body (RIGU) restrains
 O5, N2, C15, C16, C17, O5X, N2X, C15X, C16X, C17X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{O5, N2, C15, C16, C17} sigma for 1-2: 0.02, 1-3: 0.04
as
{O5X, N2X, C15X, C16X, C17X}
5. Others
 Sof(O5X)=Sof(N2X)=Sof(C15X)=Sof(H15X)=Sof(C16X)=Sof(H16D)=Sof(H16E)=Sof(H16F)=
 Sof(C17X)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(O5)=Sof(N2)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
6.a Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C16X(H16D,H16E,H16F), C17X(H17D,
 H17E,H17F)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C9(H9), C3(H3), C6(H6), C4(H4), C5(H5), C15(H15),
 C15X(H15X)
;
_shelx_res_checksum              88743
_olex2_submission_special_instructions 'No special instructions were received'