A quantitative transmetalation with a metal organic framework compound in a solid‒liquid interface reaction: synthesis, structure, kinetics, spectroscopy and electrochemistry
Bommakanti, Suresh; Das, Samar K.; CrystEngComm 21 (2019) 2438–; doi:10.1039/C9CE00021F

data_7232409
_publ_section_title
;
 A quantitative transmetalation with a metal organic framework compound in
 a solid--liquid interface reaction: synthesis, structure, kinetics,
 spectroscopy and electrochemistry
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2438
_journal_paper_doi               10.1039/C9CE00021F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C68 H48 Cu2 N4 O11'
_chemical_formula_sum            'C68 H48 Cu2 N4 O11'
_chemical_formula_weight         1224.18
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-12-30 deposited with the CCDC.    2019-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.796(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5686(4)
_cell_length_b                   24.9419(7)
_cell_length_c                   17.0814(6)
_cell_measurement_reflns_used    15144
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4240
_cell_measurement_theta_min      2.0470
_cell_volume                     5778.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.22a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.22a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.22a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47106
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76798
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         10175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                5509
_reflns_number_total             10175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ce00021f2.cif
_cod_data_source_block           skd10a
_cod_depositor_comments
'Adding full bibliography for 7232408--7232410.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7232409