Small Molecule Activation Chemistry of Cu-Fe Heterobimetallic Complexes Toward CS2 and N2O.
Jayarathne, Upul; Parmelee, Sean R.; Mankad, Neal P.; Inorganic chemistry 53 (2014) 7730–7737; doi:10.1021/ic501054z

data_4340316
_publ_section_title
;
 Small Molecule Activation Chemistry of Cu-Fe Heterobimetallic Complexes
 Toward CS2 and N2O.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7730
_journal_page_last               7737
_journal_paper_doi               10.1021/ic501054z
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C58 H58 Cu2 Fe2 N4 O4 S4, 0.5(C7 H16)'
_chemical_formula_sum            'C61.5 H66 Cu2 Fe2 N4 O4 S4'
_chemical_formula_weight         1292.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-26
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.279(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0054(3)
_cell_length_b                   21.7671(4)
_cell_length_c                   23.9146(7)
_cell_measurement_reflns_used    19865
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6210
_cell_measurement_theta_min      3.7880
_cell_volume                     6082.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9823
_diffrn_measurement_details
;
  1 omega  -48.00   29.00   1.0000    5.2700
omega____ theta____ kappa____ phi______ frames
    -      -40.7892   37.0000 -120.0000 77

  2 omega -115.00  -20.00   1.0000    5.2700
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  -57.0000  -30.0000 95

  3 omega  -86.00   -3.00   1.0000    5.2700
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  125.0000   60.0000 83

  4 omega   10.00   37.00   1.0000    5.2700
omega____ theta____ kappa____ phi______ frames
    -       40.7892  -99.0000  -60.0000 27

  5 omega   39.00   98.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -45.0000  120.0000 59

  6 omega   31.00   89.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -30.0000  -90.0000 58

  7 omega   29.00   65.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -30.0000 -120.0000 36

  8 omega   29.00   90.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -30.0000 -180.0000 61

  9 omega   31.00  102.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000  150.0000 71

 10 omega   27.00  107.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000   60.0000 80

 11 omega   48.00   91.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -45.0000   30.0000 43

 12 omega  105.00  162.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222   45.0000 -180.0000 57

 13 omega -115.00  -11.00   1.0000    5.2700
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  -57.0000   90.0000 104

 14 omega -115.00  -11.00   1.0000    5.2700
omega____ theta____ kappa____ phi______ frames
    -      -40.7892  -57.0000 -150.0000 104

 15 omega    1.00   83.00   1.0000    5.2700
omega____ theta____ kappa____ phi______ frames
    -       40.7892  -99.0000  -30.0000 82

 16 omega -134.00  -41.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -77.0000  -30.0000 93

 17 omega   23.00  109.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222  -94.0000  -90.0000 86

 18 omega   76.00  178.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222   30.0000  120.0000 102

 19 omega   76.00  178.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222   30.0000   30.0000 102

 20 omega   73.00  178.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222   77.0000 -180.0000 105

 21 omega   46.00  178.00   1.0000   21.0600
omega____ theta____ kappa____ phi______ frames
    -      107.0222   15.0000  -60.0000 132
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1222271000
_diffrn_orient_matrix_UB_12      0.0263577000
_diffrn_orient_matrix_UB_13      -0.0166880000
_diffrn_orient_matrix_UB_21      -0.0493328000
_diffrn_orient_matrix_UB_22      -0.0651238000
_diffrn_orient_matrix_UB_23      0.0017604000
_diffrn_orient_matrix_UB_31      0.0007689000
_diffrn_orient_matrix_UB_32      0.0086457000
_diffrn_orient_matrix_UB_33      0.0640318000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58518
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.10
_diffrn_reflns_theta_min         3.80
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.202
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_correction_T_min  0.138
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.5402
_exptl_crystal_size_mid          0.1338
_exptl_crystal_size_min          0.0732
_refine_diff_density_max         1.987
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         12134
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0728P)^2^+7.6600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                10188
_reflns_number_total             12134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501054z_si_002.cif
_cod_data_source_block           neal1e
_cod_depositor_comments
'Adding full bibliography for 4340314--4340317.cif.'
_cod_original_cell_volume        6082.4(2)
_cod_original_formula_sum        'C61.50 H66 Cu2 Fe2 N4 O4 S4'
_cod_database_code               4340316
_chemical_oxdiff_formula         'Cu2 Fe2 S4 O4 N4 C58 H58'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C1S-C2S = C2S-C3S = C3S-C4S = C4S-C5S = C5S-C6S = C6S-C7S
 1.54 with sigma of 0.02
 C1S-C3S = C2S-C4S = C3S-C5S = C4S-C6S = C5S-C7S
 2.52674 with sigma of 0.04
3. Restrained planarity
 C7S, C6S, C5S, C4S, C3S, C2S, C1S
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(C1S) = Uiso(C6S) = Uiso(C7S)
5. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) C7S(0.5) H7SA(0.5) H7SB(0.5)
 H7SC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB)
6.b Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC), C7S(H7SA,H7SB,H7SC)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C18(H18), C19(H19), C22(H22), C24(H24), C31(H31), C33(H33), C39(H39),
  C40(H40), C43(H43), C45(H45), C52(H52), C54(H54)
6.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C)
;