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_7121208
_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         'C55 H65 As5 Fe'
_chemical_formula_sum            'C55 H65 As5 Fe'
_chemical_formula_weight         1156.52
_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                92.777(2)
_cell_angle_beta                 114.468(3)
_cell_angle_gamma                107.131(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4626(4)
_cell_length_b                   13.7448(3)
_cell_length_c                   16.0091(4)
_cell_measurement_reflns_used    26501
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      70.7722
_cell_measurement_theta_min      3.4285
_cell_volume                     2526.71(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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      123.00(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  -98.00   -4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  125.0000  -30.0000 94

  2 omega  -28.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939  -37.0000   90.0000 95

  3 omega   15.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939   37.0000  -90.0000 101

  4 omega   67.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   77.0000 -120.0000 91

  5 omega   22.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -77.0000   60.0000 94

  6 omega   27.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -45.0000  120.0000 44

  7 omega   26.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -45.0000   90.0000 37

  8 omega   22.00  135.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -77.0000  -90.0000 113

  9 omega   24.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429 -109.0000 -129.0000 91

 10 omega   18.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -15.0000 -120.0000 140

 11 omega   11.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939   57.0000    0.0000 104

 12 omega   11.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939   57.0000 -180.0000 104

 13 omega    7.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939   77.0000   60.0000 113

 14 omega   71.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   30.0000  120.0000 87

 15 omega   74.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   45.0000  -30.0000 84

 16 omega   71.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   61.0000 -180.0000 87

 17 omega   71.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   61.0000    0.0000 87

 18 omega   26.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429 -125.0000  -60.0000 95

 19 omega   71.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   61.0000   30.0000 87

 20 omega  -70.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939   57.0000  -60.0000 103

 21 omega  -98.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  125.0000   60.0000 96

 22 omega    7.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939   77.0000 -120.0000 113

 23 omega -162.00  -61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000   60.0000 101

 24 omega   67.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   77.0000 -150.0000 91

 25 omega   67.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   77.0000  -90.0000 91

 26 omega   67.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   77.0000  120.0000 91
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0687456000
_diffrn_orient_matrix_UB_12      -0.1163630000
_diffrn_orient_matrix_UB_13      -0.0158126000
_diffrn_orient_matrix_UB_21      0.0259310000
_diffrn_orient_matrix_UB_22      0.0123606000
_diffrn_orient_matrix_UB_23      0.1038835000
_diffrn_orient_matrix_UB_31      -0.1120651000
_diffrn_orient_matrix_UB_32      0.0247473000
_diffrn_orient_matrix_UB_33      -0.0241311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34862
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.903
_diffrn_reflns_theta_min         3.431
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.5106
_exptl_crystal_size_mid          0.3445
_exptl_crystal_size_min          0.1791
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0422P)^2^+2.7615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9430
_reflns_number_total             9516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09730a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7121207--7121210.cif.'
_cod_original_cell_volume        2526.71(13)
_cod_database_code               7121208
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C55 H65 Fe As5'
_reflns_odcompleteness_completeness 99.63
_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.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C53(H53A,H53B), C32(H32A,H32B), C52(H52A,H52B), C13(H13A,
 H13B), C14(H14A,H14B), C44(H44A,H44B), C22(H22A,H22B), C23(H23A,H23B),
 C42(H42A,H42B), C43(H43A,H43B), C24(H24A,H24B), C54(H54A,H54B), C33(H33A,H33B),
  C34(H34A,H34B)
2.b Me refined with riding coordinates:
 C55(H55A,H55B,H55C), C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C45(H45A,H45B,
 H45C), C35(H35A,H35B,H35C)
2.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C7(H7), C28(H28), C20(H20), C47(H47), C37(H37), C11(H11), C17(H17),
 C31(H31), C30(H30), C38(H38), C48(H48), C21(H21), C40(H40), C10(H10), C8(H8),
 C18(H18), C50(H50), C41(H41), C51(H51)
;
_olex2_submission_special_instructions 'No special instructions were received'