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_4344734
_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, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C49 H51 B2 F8 Fe N4 P3'
_chemical_formula_weight         1018.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     iterative
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
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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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_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: 50.1562
              2theta: 29.9095
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: 50.1562
              2theta: 29.9095
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: 50.1562
              2theta: 29.9095
;
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XtaLABmini: Fixed Chi 2 circle
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Rigaku Mercury375R (2x2 bin mode)
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_diffrn_orient_matrix_UB_31      -0.009173
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_diffrn_orient_matrix_UB_33      0.015721
_diffrn_radiation_monochromator  'Graphite Monochromator'
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_diffrn_reflns_number            51614
_diffrn_reflns_theta_full        27.5049
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.3692
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2107.7278
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.7237
_refine_diff_density_min         -0.6531
_refine_diff_density_rms         0.0945
_refine_ls_d_res_high            0.7695
_refine_ls_d_res_low             11.0092
_refine_ls_goodness_of_fit_ref   1.0432
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    89
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_refine_ls_number_reflns         11327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0432
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+3.6587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1570
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -17
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              -13
_reflns_number_gt                8918
_reflns_number_total             11327
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic5b02361_si_005.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        4940(5)
_cod_database_code               4344734
_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:
 C2(H2A,H2B), C3(H3A,H3B), C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C55(H55), C41(H41), C61(H61), C44(H44), C22(H22), C11(H11),
 C51(H51), C12(H12), C45(H45), C65(H65), C13(H13), C32(H32), C33(H33), C53(H53),
  C31(H31), C15(H15), C25(H25), C43(H43), C64(H64), C23(H23), C35(H35),
 C54(H54), C52(H52), C34(H34), C42(H42), C14(H14), C63(H63), C24(H24), C62(H62)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2N(H2NA,H2NB,H2NC), C4N(H4NA,H4NB,H4NC), C6N(H6NA,H6NB,
 H6NC), C0AA(H0AA,H0AB,H0AC)
;
_olex2_submission_special_instructions 'No special instructions were received'