Unexpected differences in the reactivity between the phosphorus and arsenic derivatives [(Cp<sup>BIG</sup>Fe)<sub>2</sub>(μ,η<sup>4:4</sup>-E<sub>4</sub>)] (E = P and As).
Heinl, S.; Timoshkin, A. Y.; Müller, J; Scheer, M.; Chemical communications (Cambridge, England) 54 (2018) 2244–2247; doi:10.1039/c7cc09730a

data_7121207
_publ_section_title
;
 Unexpected differences in the reactivity between the phosphorus and
 arsenic derivatives
 [(Cp<sup>BIG</sup>Fe)<sub>2</sub>(\m,\h<sup>4:4</sup>-E<sub>4</sub>)] (E
 = P and As).
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2244
_journal_page_last               2247
_journal_paper_doi               10.1039/c7cc09730a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C112 H130 Fe2 O2 P4'
_chemical_formula_sum            'C112 H130 Fe2 O2 P4'
_chemical_formula_weight         1743.73
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-08
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                106.698(2)
_cell_angle_beta                 103.359(2)
_cell_angle_gamma                101.267(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4226(3)
_cell_length_b                   13.5015(2)
_cell_length_c                   16.1699(3)
_cell_measurement_reflns_used    11356
_cell_measurement_temperature    123.0(3)
_cell_measurement_theta_max      66.5378
_cell_measurement_theta_min      3.5582
_cell_volume                     2425.67(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.0(3)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega  -99.00  -50.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4431  125.0000    0.0000 98

  2 omega  -48.00  131.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431    0.0000  120.0000 358

  3 omega   83.00  115.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000   16.1736 64

  4 omega   71.00   97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -180.0000 52

  5 omega  116.00  166.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -180.0000 100

  6 omega    9.00  118.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -80.0086 218

  7 omega   16.00   62.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000   16.1736 92

  8 omega   19.00   77.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  150.0000 116

  9 omega   32.00  164.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  150.0000 264

 10 omega   27.00  115.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 176

 11 omega   10.00   76.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  -30.0000 132

 12 omega   27.00  129.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  138.9714 204

 13 omega   12.00  115.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   57.0000  -90.0000 206

 14 omega    8.00  120.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   77.0000  150.0000 224

 15 omega   66.00  168.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -60.0000 204

 16 omega   60.00   85.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -150.0000 50
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1227459000
_diffrn_orient_matrix_UB_12      -0.0654428000
_diffrn_orient_matrix_UB_13      -0.0126383000
_diffrn_orient_matrix_UB_21      0.0218518000
_diffrn_orient_matrix_UB_22      -0.1023455000
_diffrn_orient_matrix_UB_23      -0.0575446000
_diffrn_orient_matrix_UB_31      0.0457622000
_diffrn_orient_matrix_UB_32      -0.0254802000
_diffrn_orient_matrix_UB_33      0.0862725000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19295
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        66.642
_diffrn_reflns_theta_max         66.642
_diffrn_reflns_theta_min         3.561
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.3415
_exptl_crystal_size_mid          0.2184
_exptl_crystal_size_min          0.1325
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         8313
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7328
_reflns_number_total             8313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09730a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7121207--7121210.cif.'
_cod_original_cell_volume        2425.67(9)
_cod_database_code               7121207
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C112 H130 Fe2 P4 O2'
_chemical_oxdiff_usercomment     'Butterfly mit Cyanoalkin'
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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. Uiso/Uaniso restraints and constraints
C52B \\sim C53B \\sim C54B \\sim C55B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01
Uanis(C46) \\sim Ueq, Uanis(C46B) \\sim Ueq, Uanis(C47B) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: C46(0.65) C47(0.65) H47(0.65) C48(0.65) H48(0.65) C49(0.65)
 H49(0.65) C50(0.65) H50(0.65) C51(0.65) C52(0.65) H52A(0.65) H52B(0.65)
 C53(0.65) H53A(0.65) H53B(0.65) C54(0.65) H54A(0.65) H54B(0.65) C55(0.65)
 H55A(0.65) H55B(0.65) H55C(0.65) C46B(0.35) C47B(0.35) H47B(0.35) C48B(0.35)
 H48B(0.35) C49B(0.35) H49B(0.35) C50B(0.35) H50B(0.35) C51B(0.35) C52B(0.35)
 H52C(0.35) H52D(0.35) C53B(0.35) H53C(0.35) H53D(0.35) C54B(0.35) H54C(0.35)
 H54D(0.35) C55B(0.35) H55D(0.35) H55E(0.35) H55F(0.35) P1(0.5) P2(0.5) P3(0.5)
 P4(0.5) C57(0.5) O2(0.5) C56(0.5) O1(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C52B(H52C,H52D), C53B(H53C,H53D), C54B(H54C,H54D)
4.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C45(H45A,H45B,
 H45C), C55(H55A,H55B,H55C), C55B(H55D,H55E,H55F)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C17(H17), C18(H18), C19(H19), C20(H20),
 C27(H27), C28(H28), C29(H29), C30(H30), C37(H37), C38(H38), C39(H39), C40(H40),
  C47(H47), C48(H48), C49(H49), C50(H50), C47B(H47B), C48B(H48B), C49B(H49B),
 C50B(H50B)
;
_olex2_submission_special_instructions 'No special instructions were received'