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_7038044
_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 Cl2 Co N5, C6 H6'
_chemical_formula_sum            'C55 H56 Cl2 Co N5'
_chemical_formula_weight         916.88
_chemical_name_systematic
;
? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90.00
_cell_angle_beta                 91.1198(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7605(5)
_cell_length_b                   17.6571(6)
_cell_length_c                   17.8623(5)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.57
_cell_volume                     4654.5(3)
_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  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      104.86
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd99da
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            122537
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9516
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1928
_exptl_crystal_id                cd99da
_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 4 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.074
_refine_diff_density_max         2.369
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10300
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+8.8115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                8943
_reflns_number_total             10300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04723d2.cif
_cod_data_source_block           cd99da
_cod_depositor_comments
'Adding full bibliography for 7038039--7038044.cif.'
_cod_database_code               7038044
_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
C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C50A \\sim C51A
\\sim C52A \\sim C53A \\sim C54A \\sim C55A: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Same fragment restrains
{C50, C51, C52, C53, C54, C55} sigma for 1-2: 0.02, 1-3: 0.04
as
{C50A, C51A, C52A, C53A, C54A, C55A}
4. Others
 Sof(C50A)=Sof(H1)=Sof(C51A)=Sof(H2)=Sof(C52A)=Sof(H3)=Sof(C53A)=Sof(H4)=
 Sof(C54A)=Sof(H5)=Sof(C55A)=Sof(H6)=1-FVAR(1)
 Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=
 Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C27(HN), C30(HU), C39(H4AA), C42(H1BA)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H), C4(HA), C5(HB), C6(HC), C9(HD), C10(HE), C11(HF), C15(HG), C16(HH),
 C17(HI), C18(HJ), C23(HK), C24(HL), C25(HM), C35(H1AA), C36(H2AA), C37(H3AA),
 C45(H8BA), C46(H9BA), C47(H0CA), C48(H1CA), C49(H2CA), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C55(H55), C50A(H1), C51A(H2), C52A(H3), C53A(H4),
  C54A(H5), C55A(H6)
5.c Idealised Me refined as rotating group:
 C28(HO,HP,HQ), C29(HR,HS,HT), C31(HV,HW,HX), C32(HY,HZ,H0AA), C40(H5AA,H6AA,
 H7AA), C41(H8AA,H9AA,H0BA), C43(H2BA,H3BA,H4BA), C44(H5BA,H6BA,H7BA)
;
_olex2_submission_special_instructions 'No special instructions were received'