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_4344737
_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 Cl2 Fe P3 Si'
_chemical_formula_sum            'C40 H39 Cl2 Fe P3 Si'
_chemical_formula_weight         767.51
_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_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-26
_audit_creation_method
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Olex2 1.2
(compiled 2014.06.23 svn.r2948 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
????
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_cell_angle_alpha                93.560(8)
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_cell_length_b                   9.463(7)
_cell_length_c                   12.799(9)
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_computing_cell_refinement
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CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
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CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
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CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
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_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., 2013)'
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.9681
_diffrn_measured_fraction_theta_max 0.9681
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 50.1781
              2theta: 29.9014
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 120.0000
                 XTD: 50.1781
              2theta: 29.9014
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 240.0000
                 XTD: 50.1781
              2theta: 29.9014
;
_diffrn_measurement_device
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XtaLABmini: Fixed Chi 2 circle
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_diffrn_measurement_device_type
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Rigaku Mercury375R (2x2 bin mode)
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_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
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_diffrn_orient_matrix_UB_23      0.102852
_diffrn_orient_matrix_UB_31      0.034054
_diffrn_orient_matrix_UB_32      0.074645
_diffrn_orient_matrix_UB_33      -0.023006
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
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_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8788
_diffrn_reflns_theta_full        25.6923
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.74
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.3262
_exptl_crystal_description       Prism
_exptl_crystal_F_000             399.1456
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.1714
_refine_diff_density_min         -0.2883
_refine_diff_density_rms         0.0426
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.050(10)
_refine_ls_d_res_high            0.8197
_refine_ls_d_res_low             11.7357
_refine_ls_goodness_of_fit_ref   0.9599
_refine_ls_matrix_type           full
_refine_ls_number_constraints    73
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9599
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.940
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                6675
_reflns_number_total             7096
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic5b02361_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        961.0(12)
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               4344737
_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), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C32(H32), C31(H31), C35(H35), C43(H43), C64(H64), C42(H42),
 C65(H65), C41(H41), C11(H11), C14(H14), C12(H12), C15(H15), C61(H61), C63(H63),
  C62(H62), C34(H34), C33(H33), C25(H25), C55(H55), C21(H21), C22(H22),
 C51(H51), C54(H54), C24(H24), C45(H45), C53(H53), C23(H23), C52(H52), C44(H44)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'