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_7038041
_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         'C43 H38 Cl Co N5, 3(C4 H8 O)'
_chemical_formula_sum            'C51 H54 Cl Co N5 O2'
_chemical_formula_weight         863.07
_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             2015-01-28
_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                 98.680(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4441(18)
_cell_length_b                   20.502(3)
_cell_length_c                   16.521(2)
_cell_measurement_reflns_used    5465
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.67
_cell_measurement_theta_min      2.26
_cell_volume                     4836.4(11)
_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
; 
PUT ORTEP and POV Ray Reference here 
;
_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      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  cm69jsaq2
_diffrn_reflns_av_R_equivalents  0.2096
_diffrn_reflns_av_unetI/netI     0.1296
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8946
_diffrn_reflns_theta_full        25.63
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         1.43
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  0.2456
_exptl_absorpt_correction_T_min  0.0936
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1819
_exptl_crystal_id                cm69jsaq2
_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 -1 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         8946
_refine_ls_number_restraints     410
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                5705
_reflns_number_total             8946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04723d2.cif
_cod_data_source_block           cm69jsaq
_cod_depositor_comments
'Adding full bibliography for 7038039--7038044.cif.'
_cod_original_cell_volume        4836.5(11)
_cod_database_code               7038041
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Restrained distances 
 O2A-C50A = O2A-C49A = O2-C50 = O2-C49 
 2.32 with sigma of 0.04 
 C51A-C49A = C48-C50 = C51-C49 = C48A-C50A 
 2.46 with sigma of 0.04 
 C37A-C33 \\sim C37-C33 
 with sigma of 0.01 
 O2-C51 \\sim O2-C48 
 with sigma of 0.02 
 C51-C50 \\sim C49-C48 
 with sigma of 0.02 
 O2A-C51A \\sim O2A-C48A 
 with sigma of 0.02 
 O1-C44 \\sim O1-C47 \\sim O1A-C44A \\sim O1A-C47A 
 with sigma of 0.01 
 C44-C45 \\sim C44A-C45A \\sim C46-C47 \\sim C46-C47A 
 with sigma of 0.01 
 C45-C46 \\sim C45A-C46A 
 with sigma of 0.01 
 C51A-C50A \\sim C49A-C48A 
 with sigma of 0.02 
3. Uiso/Uaniso restraints and constraints 
C37 \\sim C37A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 
0.02 
O2 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim O2A \\sim C48A \\sim C49A 
\\sim C50A \\sim C51A: within 1.7A with sigma of 0.01 and sigma for terminal 
atoms of 0.02 
C45 \\sim C46 \\sim C44 \\sim C47 \\sim O1 \\sim C45A \\sim C46A \\sim C44A 
\\sim C47A \\sim O1A: within 1.7A with sigma of 0.01 and sigma for terminal 
atoms of 0.02 
Uanis(O2) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) 
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(C48A) \\sim Ueq, 
Uanis(C49A) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C51A) \\sim Ueq: with sigma 
of 0.1 and sigma for terminal atoms of 0.2 
Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C47) 
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C45A) \\sim Ueq, Uanis(C46A) \\sim Ueq, 
Uanis(C44A) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma 
of 0.01 and sigma for terminal atoms of 0.02 
4. Others 
 Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1) 
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1) 
 Sof(O2A)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=Sof(H49C)=Sof(H49D)= 
 Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=1-FVAR(2) 
 Sof(O2)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)= 
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=FVAR(2) 
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C44A)= 
 Sof(H44C)=Sof(H44D)=Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(O1A)=1-FVAR(3) 
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C44)=Sof(H44A)= 
 Sof(H44B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(O1)=FVAR(3) 
5.a Secondary CH2 refined with riding coordinates: 
 C45(H45A,H45B), C46(H46A,H46B), C44(H44A,H44B), C47(H47A,H47B), C45A(H45C, 
 H45D), C46A(H46C,H46D), C44A(H44C,H44D), C47A(H47C,H47D), C48(H48A,H48B), 
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C48A(H48C,H48D), C49A(H49C, 
 H49D), C50A(H50C,H50D), C51A(H51C,H51D) 
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), C25(H25), C32(H32), C34(H34), 
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43) 
5.c Idealised Me refined as rotating group: 
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C36(H36A,H36B, 
 H36C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C37A(H37D,H37E,H37F) 
;
_olex2_submission_special_instructions 'No special instructions were received'