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_7038043
_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_moiety
; 
C49 H50 Cl Co N5, 3(C4 H8 O) 
;
_chemical_formula_sum            'C49 H50 Cl Co N5'
_chemical_formula_weight         803.32
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-17
_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                90.00
_cell_angle_beta                 121.969(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.876(3)
_cell_length_b                   15.1289(11)
_cell_length_c                   22.0454(17)
_cell_measurement_reflns_used    9540
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.69
_cell_volume                     10433.7(14)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_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, 2013)'
_computing_structure_refinement
;
SHELX-2014-6 (Sheldrick, 2014)
Olex2 1.2.6 (Dolomanov et. al., 2009)
;
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker Kappa.ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm49f
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30721
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.30
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_meas      1.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3384
_exptl_crystal_id                cm49f
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-3 2 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         9540
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                6003
_reflns_number_total             9540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04723d2.cif
_cod_data_source_block           cm49f
_cod_depositor_comments
'Adding full bibliography for 7038039--7038044.cif.'
_cod_original_cell_volume        10433.6(14)
_cod_database_code               7038043
_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. Restrained distances 
 C22-C27 \\sim C22-C27A 
 with sigma of 0.02 
 C34-C39 \\sim C34-C39A 
 with sigma of 0.02 
3. Uiso/Uaniso restraints and constraints 
C27 \\sim C28 \\sim C29 \\sim C27A \\sim C28A \\sim C29A: within 1.7A with 
sigma of 0.01 and sigma for terminal atoms of 0.02 
C39 \\sim C40 \\sim C41 \\sim C39A \\sim C40A \\sim C41A: within 1.7A with 
sigma of 0.01 and sigma for terminal atoms of 0.02 
4. Same fragment restrains 
{C27, C28, C29} sigma for 1-2: 0.02, 1-3: 0.04 
as 
{C27A, C28A, C29A} 
{C39, C40, C41} sigma for 1-2: 0.02, 1-3: 0.04 
as 
{C39A, C40A, C41A} 
5. Others 
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)= 
 Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1) 
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)= 
 Sof(H29B)=Sof(H29C)=FVAR(1) 
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)= 
 Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(2) 
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)= 
 Sof(H41B)=Sof(H41C)=FVAR(2) 
6.a Ternary CH refined with riding coordinates: 
 C27(H27), C27A(H27A), C30(H30), C39(H39), C39A(H39A), C42(H42) 
6.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), C48(H48), C49(H49) 
6.c Idealised Me refined as rotating group: 
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C28A(H28D,H28E,H28F), C29A(H29D, 
 H29E,H29F), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), 
 C41(H41A,H41B,H41C), C40A(H40D,H40E,H40F), C41A(H41D,H41E,H41F), C43(H43A,
 H43B, H43C), C44(H44A,H44B,H44C) 
;
_olex2_submission_special_instructions 'No special instructions were received'