A breathing MOF: Direct crystallographic observation of the site-selective C(sp3)‒H functionalization
Shi, Dongying; Zeng, Le; Ming, Zheng; He, Cheng; Meng, Changgong; Duan, Chun-ying; RSC Adv.  (2016) –; doi:10.1039/C6RA07100G

data_7225296
_publ_section_title
;
 A breathing MOF: Direct crystallographic observation of the
 site-selective C(sp3)--H functionalization
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA07100G
_journal_year                    2016
_chemical_formula_sum            'C50 H51 Cu2 N10 O44 W10'
_chemical_formula_weight         3461.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-18 deposited with the CCDC.
2016-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                81.259(3)
_cell_angle_beta                 86.490(3)
_cell_angle_gamma                70.046(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0242(7)
_cell_length_b                   13.7795(8)
_cell_length_c                   23.9552(14)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.70
_cell_volume                     3993.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.1714
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81164
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    14.952
_exptl_absorpt_correction_T_max  0.1378
_exptl_absorpt_correction_T_min  0.1136
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3142
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.491
_refine_diff_density_min         -1.571
_refine_diff_density_rms         0.363
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         13389
_refine_ls_number_restraints     1187
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+89.0850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2181
_reflns_number_gt                9573
_reflns_number_total             13389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra07100g2.cif
_cod_data_source_block           VN@DT-DPDO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7225296