Visible light photoflow synthesis of a Cu(ii) single-chain polymer nanoparticle catalyst.
Gillhuber, Sebastian; Holloway, Joshua O.; Mundsinger, Kai; Kammerer, Jochen A.; Harmer, Jeffrey R.; Frisch, Hendrik; Barner-Kowollik, Christopher; Roesky, Peter W.; Chemical science 15 (2024) 15280–15290; doi:10.1039/d4sc03079f

data_1572416
_publ_section_title
;
 Visible light photoflow synthesis of a Cu(ii) single-chain polymer
 nanoparticle catalyst.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              15280
_journal_page_last               15290
_journal_paper_doi               10.1039/d4sc03079f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C32 H44 Cl2 Cu N4, 2(C2 H3 N)'
_chemical_formula_sum            'C36 H50 Cl2 Cu N6'
_chemical_formula_weight         701.26
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-14 deposited with the CCDC.	2024-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.905(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4097(15)
_cell_length_b                   5.8858(7)
_cell_length_c                   21.876(3)
_cell_measurement_reflns_used    11549
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.85
_cell_measurement_theta_min      1.86
_cell_volume                     1853.0(4)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_details
;
 273 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 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  0.0477
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11145
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.234
_diffrn_reflns_theta_min         1.864
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.9674
_exptl_absorpt_correction_T_min  0.8371
_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, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            'clear bluish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         4550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0565P)^2^+1.8220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3037
_reflns_number_total             4550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03079f2.cif
_cod_data_source_block           sg114
_cod_depositor_comments          'Adding full bibliography for 1572416.cif.'
_cod_database_code               1572416
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C10(H10A,H10B), C9(H9A,H9B), C2(H2C,H2D), C1(H1C,H1D)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C13(H13), C16(H16), C4(H4), C8(H8), C15(H15), C5(H5),
 C7(H7), C6(H6)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              61870
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   10.1
_stoe_evaluation_integration_b   -0.1
_stoe_evaluation_integration_ems 0.014
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 82.7
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 60.4
_stoe_evaluation_lana_max_2theta_desired 60.4
_stoe_evaluation_lana_mean_redundancy 2.4
_stoe_evaluation_lana_number_refls_after_or 11145
_stoe_evaluation_lana_number_refls_outliers 2501
_stoe_evaluation_lana_number_refls_total 13646
_stoe_evaluation_lana_number_refls_unique 4550
_stoe_evaluation_lana_number_refls_written 11145
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           6.5   12.9   19.3   25.7   32.1   38.5   44.9   51.3   57.7
<Resolution>    5.07   2.94   2.08   1.59   1.28   1.08   0.93   0.82   0.75
N(total)          66    337    889   1570   2552   2898   2660   2149    525
<Redundancy>     2.1    2.7    3.2    3.5    3.6    3.0    2.3    1.7    1.1
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0   99.6   95.3   33.9
<I/sigma>      139.8   66.2   41.7   21.4   14.9    9.9    6.3    3.2    1.8
R(int)         0.068  0.028  0.023  0.030  0.039  0.052  0.081  0.167  0.301
;
_stoe_measurement_identifier     SG114
_stoe_measurement_max_exposure_per_frame '180.0 s'
_stoe_measurement_mean_exposure_per_frame '180.0 s'
_stoe_measurement_min_exposure_per_frame '180.0 s'
_stoe_measurement_total_exposure_time '13.7 h'
_stoe_measurement_total_frame_number 273
_stoe_measurement_total_run_number 6
_stoe_measurement_tube_power     '49.8 W'