Azulenium chemistry: towards new derivatives of photochromic dihydroazulenes.
Petersen, Anne Ugleholdt; Jevric, Martyn; Elm, Jonas; Olsen, Stine T.; Tortzen, Christian G.; Kadziola, Anders; Mikkelsen, Kurt V.; Nielsen, Mogens Brøndsted; Organic & biomolecular chemistry 14 (2016) 2403–2412; doi:10.1039/c5ob02523k

data_7154911
_publ_section_title
;
 Azulenium chemistry: towards new derivatives of photochromic
 dihydroazulenes.
;
_journal_issue                   8
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2403
_journal_page_last               2412
_journal_paper_doi               10.1039/c5ob02523k
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         C28H31NSi
_chemical_formula_sum            'C28 H31 N Si'
_chemical_formula_weight         409.6456
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-09 deposited with the CCDC.
2016-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.621(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8828(6)
_cell_length_b                   19.5599(18)
_cell_length_c                   15.6723(15)
_cell_measurement_reflns_used    5519
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.46
_cell_volume                     2382.5(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      122
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 1.000
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19886
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.465
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0687 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.9253.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'drak green'
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       plade
_exptl_crystal_F_000             1070
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0402
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3277
_reflns_number_total             4215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob02523k2.cif
_cod_data_source_block           mo_d8v1275_0ma
_cod_depositor_comments
'Adding full bibliography for 7154909--7154911.cif.'
_cod_original_formula_sum        C28H31NSi
_cod_database_code               7154911
_shelxl_version_number           2014/6
_olex2_refinement_description
;
;
_shelx_res_checksum              68462