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_4344733
_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 unk
_chemical_formula_moiety         'C41 H39 Cl2 Fe P3'
_chemical_formula_sum            'C41 H39 Cl2 Fe P3'
_chemical_formula_weight         751.44
_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             2015-04-21
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                94.8155(18)
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_cell_length_b                   9.318(10)
_cell_length_c                   12.642(13)
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_computing_cell_refinement
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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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CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
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_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: 50.2255
              2theta: 29.9283
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: 50.2255
              2theta: 29.9283
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: 50.2255
              2theta: 29.9283
;
_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'
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_diffrn_orient_matrix_UB_32      -0.082356
_diffrn_orient_matrix_UB_33      -0.001523
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0718
_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            9162
_diffrn_reflns_theta_full        26.4084
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.3251
_exptl_crystal_description       Prism
_exptl_crystal_F_000             391.0685
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.3278
_refine_diff_density_min         -0.3336
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_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.022(13)
_refine_ls_d_res_high            0.7990
_refine_ls_d_res_low             11.5821
_refine_ls_goodness_of_fit_ref   0.8984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    73
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8984
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.937
_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                6735
_reflns_number_total             7487
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic5b02361_si_006.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_sg_symbol_Hall     ' P 1'
_cod_database_code               4344733
_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:
 C5(H5A,H5B), C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33), C63(H63), C12(H12), C22(H22), C11(H11), C35(H35),
 C14(H14), C32(H32), C13(H13), C15(H15), C21(H21), C51(H51), C55(H55), C52(H52),
  C65(H65), C44(H44), C54(H54), C43(H43), C41(H41), C61(H61), C42(H42),
 C64(H64), C62(H62), C34(H34), C25(H25), C24(H24), C23(H23), C53(H53), C45(H45)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'