Surface Immobilized Cu-1,10-Phenanthroline Complexes with α-Aminophosphonate Groups in the 5-Position as Heterogenous Catalysts for Efficient Atom-Transfer Radical Cyclizations
Maier, Sarah E.; Bunjaku, Osman; Kaya, Elif; Dyballa, Michael; Frey, Wolfgang; Estes, Deven; Dalton Transactions  (2023) –; doi:10.1039/D3DT01467C

data_7713213
_publ_section_title
;
 Surface Immobilized Cu-1,10-Phenanthroline Complexes with
 \a-Aminophosphonate Groups in the 5-Position as Heterogenous Catalysts
 for Efficient Atom-Transfer Radical Cyclizations
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01467C
_journal_year                    2023
_chemical_formula_moiety         'C23 H24 N3 O3 P, H2 O'
_chemical_formula_sum            'C23 H26 N3 O4 P'
_chemical_formula_weight         439.44
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-04-04 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.129(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2497(10)
_cell_length_b                   15.9458(14)
_cell_length_c                   12.3290(9)
_cell_measurement_reflns_used    3010
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      26.423
_cell_measurement_theta_min      1.833
_cell_volume                     2183.6(3)
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      145(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17088
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_min         1.833
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.706
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4476
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0777P)^2^+0.4129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3010
_reflns_number_total             4476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01467c2.cif
_cod_data_source_block           tech08
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7713213
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              89890
_shelx_hkl_checksum              72018