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_4344731
_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         'Br4 Fe, C47 H48 Fe N3 P3, 3(C2 H3 N)'
_chemical_formula_sum            'C53 H57 Br4 Fe2 N6 P3'
_chemical_formula_weight         1302.30
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-21
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
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_cell_angle_alpha                90.00
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_cell_length_a                   31.1772(10)
_cell_length_b                   13.33897(12)
_cell_length_c                   17.8988(6)
_cell_measurement_reflns_used    14063
_cell_measurement_temperature    104.40(14)
_cell_measurement_theta_max      73.9520
_cell_measurement_theta_min      3.7750
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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)
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_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)
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_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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_diffrn_ambient_environment      N~2~
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_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -37.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302  -77.0000  150.0000 112

  2 omega  -33.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302  -46.0000  -13.0000 102

  3 omega   15.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302   37.0000  -90.0000 102

  4 omega   34.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000   90.0000 43

  5 omega   30.00  142.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -77.0000  120.0000 112

  6 omega   31.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000 -120.0000 38

  7 omega   34.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000    0.0000 43

  8 omega   34.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000  -60.0000 43

  9 omega   34.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000  -90.0000 43

 10 omega   33.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562 -125.0000   60.0000 89

 11 omega   81.00  158.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   45.0000  -90.0000 77

 12 omega   34.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000   30.0000 43

 13 omega   34.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000  150.0000 43

 14 omega -115.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000   90.0000 103

 15 omega    4.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302   88.0000  176.7316 29

 16 omega    8.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302   77.0000    0.0000 112

 17 omega   78.00  158.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   30.0000    0.0000 80

 18 omega   78.00  158.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   30.0000 -180.0000 80
;
_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      -0.0186120000
_diffrn_orient_matrix_UB_12      -0.1100552000
_diffrn_orient_matrix_UB_13      -0.0119488000
_diffrn_orient_matrix_UB_21      -0.0330914000
_diffrn_orient_matrix_UB_22      0.0053821000
_diffrn_orient_matrix_UB_23      -0.1127288000
_diffrn_orient_matrix_UB_31      0.0541493000
_diffrn_orient_matrix_UB_32      -0.0344774000
_diffrn_orient_matrix_UB_33      0.0205219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19660
_diffrn_reflns_theta_full        74.12
_diffrn_reflns_theta_max         74.12
_diffrn_reflns_theta_min         3.79
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.936
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_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         8932
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+9.0838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                8651
_reflns_number_total             8932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02361_si_008.cif
_cod_data_source_block           ap79
_cod_original_cell_volume        5563.5(3)
_cod_database_code               4344731
_chemical_oxdiff_formula         'C H P Fe Br'
_reflns_odcompleteness_completeness 99.98
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C65(H65), C61(H61), C64(H64), C42(H42), C31(H31), C15(H15),
 C62(H62), C41(H41), C14(H14), C34(H34), C33(H33), C44(H44), C11(H11), C13(H13),
  C43(H43), C32(H32), C63(H63), C45(H45), C12(H12), C24(H24), C25(H25),
 C21(H21), C23(H23), C54(H54), C55(H55), C22(H22), C51(H51), C52(H52), C53(H53)
2.c Idealised Me refined as rotating group:
 C2N(H2NA,H2NB,H2NC), C6N(H6NA,H6NB,H6NC), C4N(H4NA,H4NB,H4NC), C5(H5A,H5B,
 H5C), C12N(H12A,H12B,H12C), C8N(H,HA,HB), C10N(HC,HD,HE)
;
_olex2_submission_special_instructions 'No special instructions were received'