Unprecedented copper(II) mediated in situ formation of gem-diol binuclear complexes: A combined experimental and computational study
Patel, Ram Niwas; Singh, Yogendra Pratap; Singh, Yogendra; Butcher, R. J; Zeller, Matthias; RSC Adv.  (2016) –; doi:10.1039/C6RA20367A

data_7227003
_publ_section_title
;
 Unprecedented copper(II) mediated in situ formation of gem-diol binuclear
 complexes: A combined experimental and computational study
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA20367A
_journal_year                    2016
_chemical_formula_moiety         'C48 H40 Cu2 N4 O7, 2(N O3) '
_chemical_formula_sum            'C48 H40 Cu2 N6 O13'
_chemical_formula_weight         1035.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-28 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1632(14)
_cell_length_b                   14.0696(12)
_cell_length_c                   18.5365(15)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.474
_cell_measurement_theta_min      2.236
_cell_volume                     4653.1(7)
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker Apex 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34084
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         32.104
_diffrn_reflns_theta_min         2.042
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.280
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         14843
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0628P)^2^+1.4672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10817
_reflns_number_total             14843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra20367a2.cif
_cod_data_source_block           shelx
_cod_database_code               7227003
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              73117
_shelx_fab_checksum              53250