Synthesis and structure of new vinylcoppersiloxanes and stereoregular organocyclosilsesquioxanes based on them
Frank, Inga V.; Shakirova, Albina R.; Peregudov, Alexander S.; Dolgushin, Fedor M.; Shchegolikhina, Olga I.; Anisimov, Anton A.; New Journal of Chemistry 49 (2025) 11273–11284; doi:10.1039/D5NJ01899D

data_7063833
_publ_section_title
;
 Synthesis and structure of new vinylcoppersiloxanes and stereoregular
 organocyclosilsesquioxanes based on them
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11273
_journal_page_last               11284
_journal_paper_doi               10.1039/D5NJ01899D
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C40 H48 Cu6 N4 O22 Si10, 4(C2 H6 O)'
_chemical_formula_sum            'C48 H72 Cu6 N4 O26 Si10'
_chemical_formula_weight         1783.23
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-04-15 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3540(4)
_cell_length_b                   14.1562(5)
_cell_length_c                   20.9902(7)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.20
_cell_measurement_theta_min      2.44
_cell_volume                     3618.7(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            56512
_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         29.999
_diffrn_reflns_theta_min         2.206
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  0.4355
_exptl_absorpt_correction_T_min  0.3486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       prism
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.941
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         10555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0699P)^2^+9.4659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8396
_reflns_number_total             10555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01899d2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7063833--7063836.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7063833
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.571
_shelx_estimated_absorpt_t_max   0.798
_shelx_res_checksum              3752