Activation of O2 Across a C(sp3)-C(sp3) Bond
Kumar, Rahul; Richter, Stefan; Maity, Suvendu; Sarkar, Pallavi; Chrysochos, Nicolas Dr.; Pati, Swapan K.; Ghosh, Prasanta; Schulzke, Carola; Jana, Anukul; Chemical Communications  (2022) –; doi:10.1039/D2CC00110A

data_7129577
_publ_section_title
;
 Activation of O2 Across a C(sp3)-C(sp3) Bond
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00110A
_journal_year                    2022
_chemical_formula_moiety         'C30 H30 N2 O2'
_chemical_formula_sum            'C30 H30 N2 O2'
_chemical_formula_weight         450.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-10-23 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.214(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0368(6)
_cell_length_b                   17.3714(5)
_cell_length_c                   17.3317(7)
_cell_measurement_reflns_used    12193
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.5440
_cell_measurement_theta_min      2.8320
_cell_volume                     4972.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2016 (Sheldrick, 2015)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36487
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.749
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.929
_diffrn_reflns_theta_min         2.703
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.217
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 2798 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         9847
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.1283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    0.772
_reflns_Friedel_fraction_max     0.589
_reflns_number_gt                7692
_reflns_number_total             9847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00110a2.cif
_cod_data_source_block           AJ2019
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               7129577
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              83950