Controlled Flexible Coordination in Tripodal Iron(II) Phosphane Complexes: Effects on Reactivity.
Petuker, Anette; Merz, Klaus; Merten, Christian; Apfel, Ulf-Peter; Inorganic chemistry 55 (2016) 1183–1191; doi:10.1021/acs.inorgchem.5b02361

data_4344732
_publ_section_title
;
 Controlled Flexible Coordination in Tripodal Iron(II) Phosphane
 Complexes: Effects on Reactivity.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1183
_journal_page_last               1191
_journal_paper_doi               10.1021/acs.inorgchem.5b02361
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H39 Br2 Fe P3 Si'
_chemical_formula_sum            'C40 H39 Br2 Fe P3 Si'
_chemical_formula_weight         856.38
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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_creation_date             2015-04-22
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
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_cell_formula_units_Z            1
_cell_length_a                   9.4197(3)
_cell_length_b                   9.4229(3)
_cell_length_c                   12.7283(3)
_cell_measurement_reflns_used    14603
_cell_measurement_temperature    104.7(10)
_cell_measurement_theta_max      74.0330
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_measurement_details
;
  1 omega  -75.00   37.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552   77.0000    0.0000 112

  2 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -57.0000 -120.0000 103

  3 omega  -20.00   83.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3552  -99.0000  150.0000 103

  4 omega   33.00  122.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562 -125.0000 -180.0000 89

  5 omega   24.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -94.0000  -60.0000 85

  6 omega   34.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -61.0000  -30.0000 105

  7 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   30.0000  -60.0000 80

  8 omega   81.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   45.0000   90.0000 77

  9 omega   34.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000 -180.0000 43

 10 omega   81.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   45.0000   30.0000 77

 11 omega   24.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -94.0000 -150.0000 85

 12 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000  -30.0000 80

 13 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -57.0000  150.0000 103

 14 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -57.0000  -30.0000 103

 15 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000   90.0000 112

 16 omega   75.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  120.0000 83

 17 omega   31.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000  -90.0000 38

 18 omega   75.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000 -150.0000 83

 19 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000  -60.0000 80

 20 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000   60.0000 80

 21 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   30.0000 -150.0000 80

 22 omega -124.00  -79.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -99.0000   60.0000 45

 23 omega    8.00  120.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3552   77.0000   30.0000 112

 24 omega  -35.00   68.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3552  -37.0000 -150.0000 103

 25 omega   75.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000 -120.0000 83

 26 omega   75.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  150.0000 83

 27 omega   75.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000 -180.0000 83

 28 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000   30.0000 80

 29 omega   75.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  -30.0000 83

 30 omega   75.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000   90.0000 83

 31 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000  120.0000 112

 32 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000 -150.0000 112

 33 omega  -35.00   68.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3552  -37.0000   30.0000 103

 34 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000 -150.0000 80

 35 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000  -90.0000 80

 36 omega   78.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000   90.0000 80

 37 omega   78.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   61.0000  150.0000 47

 38 omega   34.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000  120.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1343984000
_diffrn_orient_matrix_UB_12      0.1088187000
_diffrn_orient_matrix_UB_13      0.1078068000
_diffrn_orient_matrix_UB_21      0.0812446000
_diffrn_orient_matrix_UB_22      -0.1165854000
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_diffrn_orient_matrix_UB_32      0.1085362000
_diffrn_orient_matrix_UB_33      -0.0622029000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_l_min       -15
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_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
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_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.685
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6887
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_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0195
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.5587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_database_code               4344732
_reflns_odcompleteness_completeness 99.77
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_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.a Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C11(H11a,H11b), C12(H12a,H12b)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C15(H15), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
 C44(H44), C46(H46), C48(H48), C51(H51), C52(H52), C53(H53), C0AA(H0AA)
2.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c)
;
_olex2_submission_special_instructions 'No special instructions were received'