Electrochemical Properties and CO<sub>2</sub>-Reduction Ability of m-Terphenyl Isocyanide Supported Manganese Tricarbonyl Complexes.
Agnew, Douglas W.; Sampson, Matthew D.; Moore, Curtis E.; Rheingold, Arnold L.; Kubiak, Clifford P.; Figueroa, Joshua S.; Inorganic chemistry 55 (2016) 12400–12408; doi:10.1021/acs.inorgchem.6b02299

data_4349284
_publ_section_title
;
 Electrochemical Properties and CO<sub>2</sub>-Reduction Ability of
 m-Terphenyl Isocyanide Supported Manganese Tricarbonyl Complexes.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12400
_journal_page_last               12408
_journal_paper_doi               10.1021/acs.inorgchem.6b02299
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C65 H74 I Mn N2 O3, 2(C4 H8 O)'
_chemical_formula_sum            'C73 H90 I Mn N2 O5'
_chemical_formula_weight         1257.30
_chemical_name_common            IMn(CO)3(CNArDipp2)2(C4H8O)
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.184(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7392(14)
_cell_length_b                   17.0282(14)
_cell_length_c                   24.298(2)
_cell_measurement_reflns_used    8030
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.24
_cell_volume                     6769.9(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'BRUKER APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43624
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.410
_diffrn_reflns_theta_min         2.041
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0435 after correction.
The Ratio of minimum to maximum transmission is 0.8282.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_recrystallization_method 'from THF at -40C'
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.750
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         12422
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+11.5356P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8759
_reflns_number_total             12422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02299_si_002.cif
_cod_data_source_block           jfig945
_cod_original_cell_volume        6770.0(10)
_cod_database_code               4349284
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.869
_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
 O3-C65
 1.29 with sigma of 0.02
 O4-C66
 1.29 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(O2)
Uanis(C66) = Uanis(O4)
Uanis(O4) = Uanis(C66) = Uanis(C65) = Uanis(O3)
Uanis(C48) = Uanis(C48A) = Uanis(C49A) = Uanis(C49)
4. Others
 Sof(H47A)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49A)=Sof(H49D)=
 Sof(H49E)=Sof(H49F)=1-FVAR(1)
 Sof(H47)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=FVAR(1)
 Fixed Sof: I1(0.7) I2(0.3) C65(0.7) O3(0.7) C66(0.3) O4(0.3)
5.a Ternary CH refined with riding coordinates:
 C55(H55), C20(H20), C25(H25), C62(H62), C13(H13), C47(H47), C47(H47A),
 C32(H32), C50(H50)
5.b Secondary CH2 refined with riding coordinates:
 C4S(H4SA,H4SB), C1S(H1SA,H1SB), C7S(H7SA,H7SB), C2S(H2SA,H2SB), C3S(H3SA,
 H3SB), C8S(H8SA,H8SB), C6S(H6SA,H6SB), C5S(H5SA,H5SB)
5.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C7(H7), C58(H58), C9(H9), C37(H37), C8(H8), C60(H60), C38(H38),
 C59(H59), C28(H28), C18(H18), C30(H30), C16(H16), C17(H17), C43(H43), C29(H29),
  C45(H45), C44(H44)
5.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C64(H64A,H64B,H64C), C56(H56A,H56B,H56C), C22(H22A,H22B,
 H22C), C63(H63A,H63B,H63C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C21(H21A,
 H21B,H21C), C52(H52A,H52B,H52C), C49(H49A,H49B,H49C), C33(H33A,H33B,H33C),
 C51(H51A,H51B,H51C), C14(H14A,H14B,H14C), C34(H34A,H34B,H34C), C15(H15A,H15B,
 H15C), C48(H48A,H48B,H48C), C48A(H48D,H48E,H48F), C49A(H49D,H49E,H49F)
;
_shelx_res_checksum              94940
_shelx_hkl_checksum              65717
_olex2_submission_special_instructions 'No special instructions were received'