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_1572432
_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_moiety         'C43 H58 O3 W'
_chemical_formula_sum            'C43 H0.25 O3 W'
_chemical_formula_weight         748.53
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-05 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.471(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2551(6)
_cell_length_b                   14.4674(7)
_cell_length_c                   20.7849(10)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.44
_cell_volume                     3661.7(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 Venture with PHOTON III'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            97426
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.336
_diffrn_reflns_theta_min         1.972
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.189
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.3737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0751 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.8669.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       plate
_exptl_crystal_F_000             1425
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+3.7655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7736
_reflns_number_total             9139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04411h1.cif
_cod_data_source_block           hurst4
_cod_depositor_comments
'Adding full bibliography for 1572430--1572432.cif.'
_cod_database_code               1572432
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C42(H42A,H42B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C36(H36A,H36B), C35(H35A,H35B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C16(H16), C8(H8), C5(H5), C3(H3), C15(H15), C9(H9), C14(H14), C4(H4)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C20(H20A,H20B,H20C), C31(H31A,
 H31B,H31C), C30(H30A,H30B,H30C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              43886
_shelx_hkl_checksum              90180
_olex2_submission_special_instructions 'No special instructions were received'