Oriented assembly of copper metal‒organic framework membranes as tandem catalysts to enhance C‒H hydroxyalkynylation reactions with regiocontrol
Huang, Chao; Zhu, Kaifang; Lu, Guizhen; Zhang, Yingying; Wang, Dandan; Zhang, Dianbo; Mi, Liwei; Hou, Hongwei; CrystEngComm 22 (2020) 802–810; doi:10.1039/C9CE01719D

data_7239725
_publ_section_title
;
 Oriented assembly of copper metal--organic framework membranes as tandem
 catalysts to enhance C--H hydroxyalkynylation reactions with regiocontrol
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              802
_journal_page_last               810
_journal_paper_doi               10.1039/C9CE01719D
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C31 H22 Cu N4 O6'
_chemical_formula_sum            'C31 H22 Cu N4 O6'
_chemical_formula_weight         610.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-09-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-09-14 deposited with the CCDC.	2019-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8376(2)
_cell_length_b                   19.8062(4)
_cell_length_c                   11.5994(3)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.60
_cell_volume                     2714.60(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30714
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.599
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0665 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.9645.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.522
_refine_diff_density_min         -1.713
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5032
_refine_ls_number_restraints     613
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0697
_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^)+(0.1096P)^2^+10.1671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4356
_reflns_number_total             5032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01719d2.cif
_cod_data_source_block           mo_20181206a_0ma_b
_cod_depositor_comments
;Adding full bibliography for 7239725.cif.

 Adding full bibliography for 7239725.cif.
;
_cod_database_code               7239725
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.005 and
sigma for terminal atoms of 0.01
4.a Rotating group:
 O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12),
 C13(H13), C15(H15), C17(H17), C19(H19), C22(H22), C23(H23), C26(H26), C28(H28),
  C29(H29), C30(H30), C31(H31)
;
_shelx_res_checksum              24943
_olex2_submission_special_instructions 'No special instructions were received'