A new generation of terminal copper nitrenes and their application in aromatic C-H amination reactions.
Thomas, Fabian; Oster, Matthias; Schön, Florian; Göbgen, Kai C; Amarouch, Benedikt; Steden, Dominik; Hoffmann, Alexander; Herres-Pawlis, Sonja; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6444–6462; doi:10.1039/d1dt00832c

data_7707181
_publ_section_title
;
 A new generation of terminal copper nitrenes and their application in
 aromatic C-H amination reactions.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6444
_journal_page_last               6462
_journal_paper_doi               10.1039/d1dt00832c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C38 H29 Cl Cu N6, F6 P, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C39.5 H32 Cl4 Cu F6 N6 P'
_chemical_formula_weight         941.02
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-30 deposited with the CCDC.	2021-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                89.59(3)
_cell_angle_beta                 76.64(3)
_cell_angle_gamma                87.33(3)
_cell_formula_units_Z            4
_cell_length_a                   11.931(2)
_cell_length_b                   15.931(3)
_cell_length_c                   21.581(4)
_cell_measurement_reflns_used    15826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.87
_cell_measurement_theta_min      3.81
_cell_volume                     3986.6(13)
_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 0.753
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details      ' 3869 frames, detector distance = 65 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.1499
_diffrn_reflns_Laue_measured_fraction_full 0.753
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23297
_diffrn_reflns_point_group_measured_fraction_full 0.753
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         70.093
_diffrn_reflns_theta_min         4.613
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.205
_exptl_absorpt_correction_T_max  0.5439
_exptl_absorpt_correction_T_min  0.0028
_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            colorless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       rod
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         12881
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2177
_refine_ls_wR_factor_ref         0.2393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6383
_reflns_number_total             12881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00832c2.cif
_cod_data_source_block           C2
_cod_depositor_comments
;
Adding full bibliography for 7707179--7707183.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        3986.6(15)
_cod_original_formula_moiety     '2(C38 H29 Cl Cu N6), 2(F6 P), 3(C H2 Cl2)'
_cod_original_formula_sum        'C79 H64 Cl8 Cu2 F12 N12 P2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1882.04
_cod_database_code               7707181
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.472
_shelx_estimated_absorpt_t_max   0.730
_shelx_res_checksum              22463
_shelx_hkl_checksum              16801