A robust and efficient cobalt molecular catalyst for CO2 reduction
Sharon Lai-Fung Chan; Tsz Lung Lam; Chen Yang; Siu-Cheong Yan; Nga Man Cheng; Chem.Commun. 51 (2015) 7799–; doi:10.1039/C5cc00566C

data_7117052
_publ_section_title
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 A robust and efficient cobalt molecular catalyst for CO2 reduction
;
_journal_name_full               Chem.Commun.
_journal_page_first              7799
_journal_paper_doi               10.1039/C5cc00566C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         '1(C18 H18 Cl Co N4), Cl'
_chemical_formula_sum            'C18 H18 Cl2 Co N4'
_chemical_formula_weight         420.19
_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     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc141jqf
_audit_creation_date             2015-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2015-01-18 deposited with the CCDC.
2015-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.060(2)
_cell_angle_beta                 103.277(2)
_cell_angle_gamma                110.696(2)
_cell_formula_units_Z            6
_cell_length_a                   11.5740(6)
_cell_length_b                   15.2041(9)
_cell_length_c                   19.9081(11)
_cell_measurement_temperature    100
_cell_volume                     3176.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57557
_diffrn_reflns_theta_full        67.44
_diffrn_reflns_theta_max         67.44
_diffrn_reflns_theta_min         2.29
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.727
_exptl_absorpt_correction_T_max  0.2527
_exptl_absorpt_correction_T_min  0.0751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1715 before and 0.1301 after correction.
The Ratio of minimum to maximum transmission is 0.2972.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1290
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.594
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.426
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         11143
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.427
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.1207
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3208
_refine_ls_wR_factor_ref         0.3355
_reflns_number_gt                9371
_reflns_number_total             11143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc00566c2.cif
_cod_data_source_block           cxy129_0m
_cod_database_code               7117052
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N12) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C50) \\sim Ueq,
Uanis(C44) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C39) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl5B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C37A) = Uanis(N9) = Uanis(C41A) = Uanis(C40A) = Uanis(C39A) = Uanis(C38A)
Uanis(N10) = Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C40) = Uanis(C41)
Uanis(N14) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47)
3. Others
 Sof(N12)=Sof(C53)=Sof(C52)=Sof(H52)=Sof(C51)=Sof(H51)=Sof(C50)=Sof(H50)=
 Sof(C49)=Sof(H49)=Sof(N14)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=
 Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(C48)=Sof(H48C)=Sof(H48D)=Sof(C54)=
 Sof(H54C)=Sof(H54D)=Sof(C42)=Sof(H42C)=Sof(H42D)=Sof(C41)=Sof(C40)=Sof(H40)=
 Sof(C39)=Sof(H39)=Sof(C38)=Sof(H38)=Sof(C37)=Sof(H37)=Sof(N10)=1-FVAR(1)
 Sof(N9)=Sof(C41A)=Sof(C40A)=Sof(H40A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=Sof(H38A)=
 Sof(C37A)=Sof(H37A)=Sof(C43A)=Sof(H43A)=Sof(N13)=Sof(C47A)=Sof(C46A)=Sof(H46A)=
 Sof(C45A)=Sof(H45A)=Sof(C44A)=Sof(H44A)=Sof(C54A)=Sof(H54A)=Sof(H54B)=
 Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(N11)=Sof(C53A)=
 Sof(C52A)=Sof(H52A)=Sof(C51A)=Sof(H51A)=Sof(C50A)=Sof(H50A)=Sof(C49A)=
 Sof(H49A)=FVAR(1)
 Fixed Sof: Cl5(0.5) Cl6A(0.25) Cl6B(0.25) Cl6(0.25) Cl5B(0.5) Cl5A(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C30(H30A,H30B), C18(H18A,H18B), C24(H24A,H24B), C12(H12A,H12B),
 C36(H36A,H36B), C54A(H54A,H54B), C42A(H42A,H42B), C48A(H48A,H48B), C48(H48C,
 H48D), C54(H54C,H54D), C42(H42C,H42D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C16(H16), C19(H19), C13(H13), C1(H1), C22(H22), C14(H14),
 C20(H20), C25(H25), C21(H21), C7(H7), C4(H4), C34(H34), C32(H32), C26(H26),
 C8(H8), C31(H31), C10(H10), C15(H15), C28(H28), C27(H27), C9(H9), C33(H33),
 C40A(H40A), C39A(H39A), C38A(H38A), C37A(H37A), C43A(H43A), C46A(H46A),
 C45A(H45A), C44A(H44A), C52(H52), C51(H51), C50(H50), C49(H49), C43(H43),
 C44(H44), C45(H45), C46(H46), C40(H40), C39(H39), C38(H38), C37(H37),
 C52A(H52A), C51A(H51A), C50A(H50A), C49A(H49A)
4.c Fitted hexagon refined as free rotating group:
 C43A(N13,C47A,C46A,C45A,C44A), N12(C53,C52,C51,C50,C49), N14(C43,C44,C45,C46,
 C47), C41(C40,C39,C38,C37,N10), N11(C53A,C52A,C51A,C50A,C49A)
;
_olex2_submission_special_instructions 'No special instructions were received'