Manipulating electron transfer – the influence of substituents on novel copper guanidine quinolinyl complexes
Heck, Joshua; Metz, Fabian; Buchenau, Sören; Teubner, Melissa; Grimm-Lebsanft, Benjamin; Spaniol, Thomas P.; Hoffmann, Alexander; Rübhausen, Michael A.; Herres-Pawlis, Sonja; Chemical Science 13 (2022) 8274–8288; doi:10.1039/D2SC02910C

data_1567296
_publ_section_title
;
 Manipulating electron transfer -- the influence of substituents on novel
 copper guanidine quinolinyl complexes
;
_journal_issue                   28
_journal_name_full               'Chemical Science'
_journal_page_first              8274
_journal_page_last               8288
_journal_paper_doi               10.1039/D2SC02910C
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C32 H40 Cu N8 O4, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H46 Cu F6 N10 O10 S2'
_chemical_formula_weight         1044.51
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-06 deposited with the CCDC.	2022-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.99(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.547(3)
_cell_length_b                   12.641(3)
_cell_length_c                   26.447(5)
_cell_measurement_reflns_used    59878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.74
_cell_measurement_theta_min      1.79
_cell_volume                     4518.0(17)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.0.0 (STOE, 2018)
X-Area LANA 1.72.3.0 (STOE, 2018)
;
_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 1.82, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      ' 2359 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 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  0.0654
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            104293
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.032
_diffrn_reflns_theta_min         2.081
_diffrn_source                   'Genix Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.8507
_exptl_absorpt_correction_T_min  0.3824
_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.
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.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         15723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0551P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9100
_reflns_number_total             15723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02910c2.cif
_cod_data_source_block           C8b
_cod_original_cell_volume        4518.1(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567296
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              18420