Enhanced catalytic activity of copper complexes in microgels for aerobic oxidation of benzyl alcohols.
Schäfer, Dominic; Fink, Fabian; Kleinschmidt, Denise; Keisers, Kristina; Thomas, Fabian; Hoffmann, Alexander; Pich, Andrij; Herres-Pawlis, Sonja; Chemical communications (Cambridge, England) 56 (2020) 5601–5604; doi:10.1039/d0cc02433c

data_7126449
_publ_section_title
;
 Enhanced catalytic activity of copper complexes in microgels for aerobic
 oxidation of benzyl alcohols.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5601
_journal_page_last               5604
_journal_paper_doi               10.1039/d0cc02433c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C8 H11 Cl2 Cu N5, 0.5(H2 O)'
_chemical_formula_sum            'C8 H12 Cl2 Cu N5 O0.5'
_chemical_formula_weight         320.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-03-06 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                110.78(3)
_cell_angle_beta                 103.66(3)
_cell_angle_gamma                96.17(3)
_cell_formula_units_Z            4
_cell_length_a                   7.7357(15)
_cell_length_b                   12.816(3)
_cell_length_c                   13.522(3)
_cell_measurement_reflns_used    13336
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.50
_cell_measurement_theta_min      2.78
_cell_volume                     1190.6(6)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.131.0 (STOE, 2017)
;
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area LANA 1.71.4.0 (STOE, 2017)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.77, Darmstadt 2016
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Counting Detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details      ' 1227 frames, detector distance = 60 mm'
_diffrn_measurement_device       '4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8358
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.772
_diffrn_source                   'Genix Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.268
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.1365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       rod
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4269
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0742P)^2^+9.8173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3873
_reflns_number_total             4269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02433c2.cif
_cod_data_source_block           C1
_cod_depositor_comments
;
         Adding full bibliography for 7126449.cif.

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C16 H24 Cl4 Cu2 N10 O'
_cod_original_formula_weight         641.33
_cod_original_formula_moiety         '2(C8 H11 Cl2 Cu N5), H2 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        1190.6(5)
_cod_database_code               7126449
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.839
_exptl_absorpt_special_details
;
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_shelx_res_checksum              26027