Chromium mediated reductive coupling of isonitrile forms unusual heterocycles.
Shen, Jingmei; Yap, Glenn P. A.; Theopold, Klaus H.; Journal of the American Chemical Society 136 (2014) 3382–3384; doi:10.1021/ja501291p

data_4121491
_publ_section_title
;
 Chromium mediated reductive coupling of isonitrile forms unusual
 heterocycles.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3382
_journal_page_last               3384
_journal_paper_doi               10.1021/ja501291p
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C102 H158 Cr2 N10 O2'
_chemical_formula_weight         1660.37
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 112.616(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.418(9)
_cell_length_b                   13.005(4)
_cell_length_c                   27.439(13)
_cell_measurement_reflns_used    1019
_cell_measurement_temperature    195(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     9690(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      195(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1313
_diffrn_reflns_av_unetI/netI     0.1310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            61992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.136
_diffrn_reflns_theta_min         1.726
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.806672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_F_000             3616
_platon_squeeze_details
;

PLATON Reference : 
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
Spek, A.L. (2009). Acta Cryst. D65, 148-155.

Void space analysis consistent with initial solutions 
displaying two, severely disordered half molecules 
of diethylether solvent per asymmetric unit.
;
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         11662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_gt           0.0831
_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^)+(0.0588P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5288
_reflns_number_total             11662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja501291p_si_001.cif
_cod_data_source_block           kla0079s-sr
_cod_database_code               4121491
_shelxl_version_number           2013-4
_shelx_res_checksum              2107