Monoanionic bis(carbene) pincer complexes featuring cobalt(I-III) oxidation states.
Ibrahim, Abdulrahman D.; Tokmic, Kenan; Brennan, Marshall R.; Kim, Dongyoung; Matson, Ellen M.; Nilges, Mark J.; Bertke, Jeffery A.; Fout, Alison R.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9805–9811; doi:10.1039/c5dt04723d

data_7038042
_publ_section_title
;
 Monoanionic bis(carbene) pincer complexes featuring cobalt(I-III)
 oxidation states.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9805
_journal_page_last               9811
_journal_paper_doi               10.1039/c5dt04723d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C47 H48 Co N6'
_chemical_formula_weight         755.84
_chemical_name_systematic
; 
? 
;
_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
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-19
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_audit_update_record
;
2015-12-01 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                65.272(7)
_cell_angle_beta                 78.937(8)
_cell_angle_gamma                69.194(8)
_cell_formula_units_Z            2
_cell_length_a                   10.9123(19)
_cell_length_b                   13.358(2)
_cell_length_c                   15.720(3)
_cell_measurement_reflns_used    9520
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.4
_cell_volume                     1943.1(6)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement
; 
SHELX-2014-6 (Sheldrick, 2014) 
Olex2 1.2.6 (Dolomanov et. al., 2009) 
;
_computing_structure_solution    'SHELX-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd06h
_diffrn_reflns_av_R_equivalents  0.1320
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7133
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         2.40
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.98885
_exptl_absorpt_correction_T_min  0.93421
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             798
_exptl_crystal_id                cd06h
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 2 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7133
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+2.2662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                5598
_reflns_number_total             7133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04723d2.cif
_cod_data_source_block           cd06h
_cod_depositor_comments
'Adding full bibliography for 7038039--7038044.cif.'
_cod_original_cell_volume        1943.0(6)
_cod_database_code               7038042
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Uiso/Uaniso restraints and constraints 
C45 \\sim C46 \\sim C47 \\sim C45A \\sim C46A \\sim C47A: within 1.7A with 
sigma of 0.01 and sigma for terminal atoms of 0.02 
3. Same fragment restrains 
{C45, C46, C47} sigma for 1-2: 0.02, 1-3: 0.04 
as 
{C45A, C46A, C47A} 
4. Others 
 Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=1-FVAR(1) 
 Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=FVAR(1) 
5.a Ternary CH refined with riding coordinates: 
 C27(H27), C30(H30), C39(H39), C42(H42) 
5.b Aromatic/amide H refined with riding coordinates: 
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C15(H15), 
 C16(H16), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C35(H35), 
 C36(H36), C37(H37), C45(H45), C46(H46), C47(H47), C45A(H45A), C46A(H46A), 
 C47A(H47A) 
5.c Idealised Me refined as rotating group: 
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B, 
 H32C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), 
 C44(H44A,H44B,H44C) 
;
_olex2_submission_special_instructions 'No special instructions were received'