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_4344736
_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_formula_moiety         'C47 H48 Fe N3 P3, Cl6 Fe2, 2(C2 H3 N)'
_chemical_formula_sum            'C51 H54 Cl6 Fe3 N5 P3'
_chemical_formula_weight         1210.20
_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'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 89.866(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1885(10)
_cell_length_b                   14.8199(12)
_cell_length_c                   28.7052(19)
_cell_measurement_reflns_used    15904
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.1
_cell_volume                     5610.5(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.9898
_diffrn_measured_fraction_theta_max 0.9898
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 50.1964
              2theta: 29.9414
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 120.0000
                 XTD: 50.1964
              2theta: 29.9414
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 240.0000
                 XTD: 50.1964
              2theta: 29.9414
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Mercury375R (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.025742
_diffrn_orient_matrix_UB_12      -0.014460
_diffrn_orient_matrix_UB_13      0.069839
_diffrn_orient_matrix_UB_21      0.019027
_diffrn_orient_matrix_UB_22      0.064429
_diffrn_orient_matrix_UB_23      0.006327
_diffrn_orient_matrix_UB_31      -0.031289
_diffrn_orient_matrix_UB_32      0.007954
_diffrn_orient_matrix_UB_33      0.013091
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            66759
_diffrn_reflns_theta_full        30.5769
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.4326
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2489.6143
_exptl_crystal_recrystallization_method
'via diffusion of diethylether into a solution of acetonitrile/compound'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.7790
_refine_diff_density_min         -0.9531
_refine_diff_density_rms         0.1347
_refine_ls_d_res_high            0.6986
_refine_ls_d_res_low             10.3101
_refine_ls_goodness_of_fit_ref   1.0328
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    97
_refine_ls_number_parameters     658
_refine_ls_number_reflns         17038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0328
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.0062
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+1.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              40
_reflns_limit_l_min              0
_reflns_number_gt                13872
_reflns_number_total             17038
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic5b02361_si_007.cif
_cod_data_source_block           shelx
_cod_database_code               4344736
_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. Others
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1B)=FVAR(1)
 Sof(Cl4B)=1-FVAR(2)
 Sof(Cl4A)=FVAR(2)
 Sof(Cl2B)=1-FVAR(3)
 Sof(Cl2A)=FVAR(3)
 Sof(Fe2B)=1-FVAR(4)
 Sof(Fe2A)=FVAR(4)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C11(H11), C41(H41), C45(H45), C25(H25), C42(H42), C21(H21),
 C33(H33), C22(H22), C61(H61), C34(H34), C65(H65), C32(H32), C35(H35), C55(H55),
  C63(H63), C54(H54), C12(H12), C53(H53), C43(H43), C15(H15), C51(H51),
 C44(H44), C24(H24), C13(H13), C52(H52), C23(H23), C14(H14), C64(H64), C62(H62)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2N(H2NA,H2NB,H2NC), C4N(H4NA,H4NB,H4NC), C6N(H6NA,H6NB,
 H6NC), C8N(H8NA,H8NB,H8NC), C10N(H10A,H10B,H10C)
;
_olex2_submission_original_sample_id AP32
_olex2_submission_special_instructions 'No special instructions were received'