Homoleptic complexes of isocyano- and diisocyanobiazulenes with a 12-electron, ligand-based redox capacity
Connelly, Patrick T.; Applegate, Jason C.; Maldonado, David A.; Okeowo, Monisola K.; Henke, Wade C.; Oliver, Allen Grayson; Berrie, Cindy L.; Barybin, Mikhail V.; Dalton Transactions  (2023) –; doi:10.1039/D3DT01958F

data_7713619
_publ_section_title
;
 Homoleptic complexes of isocyano- and diisocyanobiazulenes with a
 12-electron, ligand-based redox capacity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01958F
_journal_year                    2023
_chemical_formula_moiety         'C38 H29 Cr N O13, 0.375(C H2 Cl2)'
_chemical_formula_sum            'C38.38 H29.75 Cl0.75 Cr N O13'
_chemical_formula_weight         791.47
_chemical_melting_point          428
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-06-14 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90.327(2)
_cell_angle_beta                 92.499(2)
_cell_angle_gamma                91.085(2)
_cell_formula_units_Z            4
_cell_length_a                   10.7018(5)
_cell_length_b                   16.7383(9)
_cell_length_c                   20.6013(11)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.961
_cell_measurement_theta_min      2.280
_cell_volume                     3686.1(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX 3 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            82214
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         1.563
_diffrn_source                   'fine-focus sealed-tube'
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.9753
_exptl_absorpt_correction_T_min  0.9216
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0443 before and 0.0415 after correction.
The Ratio of minimum to maximum transmission is 0.9449.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       plate
_exptl_crystal_F_000             1631
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, pentane'
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.375
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     990
_refine_ls_number_reflns         18295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+3.4981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13850
_reflns_number_total             18295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01958f2.cif
_cod_data_source_block           cmpd_7
_cod_database_code               7713619
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.905
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              28799