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_4344735
_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         'C46 H48 Fe N3 P3 Si, C4 H8 O, 2(B F4)'
_chemical_formula_sum            'C50 H56 B2 F8 Fe N3 O P3 Si'
_chemical_formula_weight         1065.45
_chemical_name_systematic
;
 ? 
;
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.265(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1059(11)
_cell_length_b                   15.7016(9)
_cell_length_c                   26.135(2)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      2.0
_cell_volume                     5255.4(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      173(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 50.2064
              2theta: 29.9213
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 120.0000
                 XTD: 50.2064
              2theta: 29.9213
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 240.0000
                 XTD: 50.2064
              2theta: 29.9213
;
_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      0.010305
_diffrn_orient_matrix_UB_12      0.033059
_diffrn_orient_matrix_UB_13      0.069985
_diffrn_orient_matrix_UB_21      0.002763
_diffrn_orient_matrix_UB_22      -0.057688
_diffrn_orient_matrix_UB_23      0.026844
_diffrn_orient_matrix_UB_31      0.038989
_diffrn_orient_matrix_UB_32      0.002881
_diffrn_orient_matrix_UB_33      0.002179
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44522
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_correction_T_min  0.9288
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         9235
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0727P)^2^+6.6513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                6693
_reflns_number_total             9235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02361_si_004.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        5255.5(7)
_cod_database_code               4344735
_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
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4A \\sim B1-F4B
 with sigma of 0.02
 B2-F5 \\sim B2-F6 \\sim B2-F7 \\sim B2-F8A \\sim B2-F8A
 with sigma of 0.02
3. Rigid bond restraints
 F1, F2, F3, F4A, F4B, F5, F6, F7, F8A, F8B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(F4B)=1-FVAR(1)
 Sof(F4A)=FVAR(1)
 Sof(F8B)=1-FVAR(2)
 Sof(F8A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C44(H44), C42(H42), C24(H24), C13(H13), C34(H34), C14(H14), C25(H25),
 C61(H61), C62(H62), C11(H11), C41(H41), C65(H65), C52(H52), C32(H32), C53(H53),
  C12(H12), C1AA(H1AA), C55(H55), C43(H43), C15(H15), C54(H54), C21(H21),
 C51(H51), C23(H23), C64(H64), C63(H63), C31(H31), C22(H22), C35(H35),
 C101(H101), C102(H102), C33(H33)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6N(H6NA,H6NB,H6NC), C2N(H2NA,H2NB,H2NC), C4N(H4NA,H4NB,
 H4NC), C100(H10A,H10B,H10C), C103(H10D,H10E,H10F)
;
_olex2_submission_original_sample_id Ap25
_olex2_submission_special_instructions 'No special instructions were received'