Accessible triplet excited states in the photoisomerization of allenes with extended conjugation.
Álvarez-García, Jonathan; García-Lago, Ramón; Alonso-Gómez, José Lorenzo; López, Carlos Silva; Cid, María Magdalena; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1357–1363; doi:10.1039/d1dt03688b

data_7709096
_publ_section_title
;
 Accessible triplet excited states in the photoisomerization of allenes
 with extended conjugation.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1357
_journal_page_last               1363
_journal_paper_doi               10.1039/d1dt03688b
_journal_volume                  51
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C49 H56 Br N2 O5 Re, C2 H3 N'
_chemical_formula_sum            'C51 H59 Br N3 O5 Re'
_chemical_formula_weight         1060.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           24
_space_group_name_Hall           'I 2b 2c'
_space_group_name_H-M_alt        'I 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-09-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-04 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6986(9)
_cell_length_b                   24.7762(14)
_cell_length_c                   26.3491(16)
_cell_measurement_reflns_used    9058
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      2.18
_cell_volume                     10248.5(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_source         'Incoatec high brillance I\muS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53772
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_min         2.595
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.196
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1354 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.6838.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       prism
_exptl_crystal_F_000             4288
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.077
_refine_diff_density_max         2.868
_refine_diff_density_min         -2.654
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.026(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         12762
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0406P)^2^+147.3653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                10251
_reflns_number_total             12762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03688b2.cif
_cod_data_source_block           32079101_0m_a
_cod_depositor_comments          'Adding full bibliography for 7709096.cif.'
_cod_database_code               7709096
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.548
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.974(19)
 0.026(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 C1-O1
 1.3 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C3)
Uanis(O3) = Uanis(O2) = Uanis(O1)
5. Others
 Fixed Sof: N1(0.5) C11(0.5) H12A(0.5) H12B(0.5) H12C(0.5) N2(0.5) C21(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C101(H101), C102(H102), C104(H104), C107(H107), C109(H109), C110(H110)
6.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C),
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C97(H97A,H97B,
 H97C), C111(H11A,H11B,H11C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C)
6.c Idealised tetrahedral OH refined as rotating group:
 O11(H11), O13(H13)
;
_shelx_res_checksum              28679
_olex2_submission_special_instructions 'No special instructions were received'