Cr(i)Cl as well as Cr+are stabilised between two cyclic alkyl amino carbenes
Samuel, Prinson P.; Neufeld, Roman; Chandra Mondal, Kartik; Roesky, Herbert W.; Herbst-Irmer, Regine; Stalke, Dietmar; Demeshko, Serhiy; Meyer, Franc; Rojisha, Vallyanga Chalil; De, Susmita; Parameswaran, Pattiyil; Stückl, A. Claudia; Kaim, Wolfgang; Christian, Jonathan H.; Bindra, Jasleen K.; Dalal, Naresh S.; Chem. Sci. 6 (2015) 3148–; doi:10.1039/C5SC00646E

data_1518882
_publ_section_title
;
 Cr(i)Cl as well as Cr+are stabilised between two cyclic alkyl amino
 carbenes
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3148
_journal_paper_doi               10.1039/C5SC00646E
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C82.50 H86 B Cr F24 N2'
_chemical_formula_sum            'C82.5 H86 B Cr F24 N2'
_chemical_formula_weight         1624.34
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-11-17 deposited with the CCDC.
2015-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                85.98(2)
_cell_angle_beta                 89.96(2)
_cell_angle_gamma                87.39(2)
_cell_formula_units_Z            2
_cell_length_a                   13.468(2)
_cell_length_b                   14.272(2)
_cell_length_c                   20.836(3)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.444
_cell_measurement_theta_min      2.301
_cell_volume                     3991.0(10)
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_collection       'APEX2 v2012.4-3'
_computing_data_reduction        'SAINT V8.30C'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'SHELXP in SHELXTL-97'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            84083
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.432
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/3
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00067(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1164
_refine_ls_number_reflns         14604
_refine_ls_number_restraints     2848
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0314P)^2^+2.3036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10948
_reflns_number_total             14604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc00646e2.cif
_cod_data_source_block           CAAC-Cr_1
_cod_depositor_comments
'Adding full bibliography for 1518882--1518884.cif.'
_cod_original_formula_sum        'C82.50 H86 B Cr F24 N2'
_cod_database_code               1518882
_shelxl_version_number           2014-3
_shelx_res_checksum              59233