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_4340314
_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         'C33 H39 Cu Fe N2 O2'
_chemical_formula_sum            'C33 H39 Cu Fe N2 O2'
_chemical_formula_weight         615.05
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-01
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.1443(2)
_cell_length_b                   17.4185(3)
_cell_length_c                   22.8343(3)
_cell_measurement_reflns_used    23080
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.1710
_cell_measurement_theta_min      3.5480
_cell_volume                     6421.22(16)
_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
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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 0.9976
_diffrn_measured_fraction_theta_max 0.9205
_diffrn_measurement_details
;
  1 omega  -16.00   70.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       11.3779   77.0000    0.0000 86

  2 omega   53.00   79.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       11.3779   74.0000  -86.0000 26

  3 omega -100.00  -75.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -      -11.7685  178.0000   30.0000 25

  4 omega  -91.00  -57.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -      -11.7685 -178.0000  150.0000 34

  5 omega  -98.00  -67.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -      -11.7685 -178.0000   90.0000 31

  6 omega  -18.00   85.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       11.3779   57.0000  120.0000 103

  7 omega  -20.00    0.00   1.0000   13.2200
omega____ theta____ kappa____ phi______ frames
    -       11.3779  -99.0000 -180.0000 20
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0260745000
_diffrn_orient_matrix_UB_12      -0.0290996000
_diffrn_orient_matrix_UB_13      0.0115502000
_diffrn_orient_matrix_UB_21      -0.0034928000
_diffrn_orient_matrix_UB_22      -0.0165758000
_diffrn_orient_matrix_UB_23      -0.0282691000
_diffrn_orient_matrix_UB_31      0.0351533000
_diffrn_orient_matrix_UB_32      -0.0231946000
_diffrn_orient_matrix_UB_33      0.0057287000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52036
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.41
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.601
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.6583
_exptl_crystal_size_mid          0.4541
_exptl_crystal_size_min          0.4484
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         8190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+3.1535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                7022
_reflns_number_total             8190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501054z_si_002.cif
_cod_data_source_block           neal1a
_cod_depositor_comments
'Adding full bibliography for 4340314--4340317.cif.'
_cod_original_cell_volume        6421.21(16)
_cod_database_code               4340314
_chemical_oxdiff_formula         'Cu Fe C33 H39 O2 N2'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C18(H18), C20(H20), C27(H27), C29(H29)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;