Snapshot of cyclooctyne ring-opening to a tethered alkylidene cyclic polymer catalyst.
Hurst, Javier M.; Yadav, Rinku; Boeck, Parker T.; Ghiviriga, Ion; Brantley, ChristiAnna L; Dobrzycki, Łukasz; Veige, Adam S.; Chemical science 15 (2024) 15873–15879; doi:10.1039/d4sc04411h

data_1572431
_publ_section_title
;
 Snapshot of cyclooctyne ring-opening to a tethered alkylidene cyclic
 polymer catalyst.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              15873
_journal_page_last               15879
_journal_paper_doi               10.1039/d4sc04411h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C43 H56 O3 W'
_chemical_formula_weight         804.72
_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     direct
_audit_update_record
;
2024-06-05 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.7480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8411(3)
_cell_length_b                   16.8936(5)
_cell_length_c                   20.2912(5)
_cell_measurement_reflns_used    12596
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      31.2619
_cell_measurement_theta_min      1.5981
_cell_volume                     3662.58(17)
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 V2019 (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    ' '
_computing_publication_material  'APEX3 V2019 (Bruker Nano, Inc., 2019)'
_computing_structure_refinement  'SHELXL2015 (Sheldrick G. M., 2019)'
_computing_structure_solution    'SHELXL2015 (Sheldrick G. M., 2019)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER D8 Venture with PHOTON III'
_diffrn_measurement_method       '\o and \f scans'
_diffrn_radiation_monochromator  'HELIOS multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            102801
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    3.192
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   'Numerical Mu From Formula'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'clear pale orange'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.130
_refine_diff_density_max         2.979
_refine_diff_density_min         -1.572
_refine_ls_extinction_coef       0.00042(8)
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         13260
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+5.4497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                12098
_reflns_number_total             13260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04411h1.cif
_cod_data_source_block           hurst6
_cod_depositor_comments
'Adding full bibliography for 1572430--1572432.cif.'
_cod_database_code               1572431
_shelx_res_checksum              31281
_shelx_hkl_checksum              60142