Triple-decker sandwich complexes with a bent cyclo-P<sub>5</sub> middle-deck.
Mädl, Eric; Peresypkina, Eugenia; Timoshkin, Alexey Y.; Scheer, Manfred; Chemical communications (Cambridge, England) 52 (2016) 12298–12301; doi:10.1039/c6cc06883a

data_7125111
_publ_section_title
;
 Triple-decker sandwich complexes with a bent cyclo-P<sub>5</sub>
 middle-deck.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12298
_journal_page_last               12301
_journal_paper_doi               10.1039/c6cc06883a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C31 H55 Co Fe P5 Si, F6 P'
_chemical_formula_sum            'C31 H55 Co F6 Fe P6 Si'
_chemical_formula_weight         870.44
_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_hydrogens   geom
_audit_creation_date             2015-04-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-08-12 deposited with the CCDC.
2016-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.95450(10)
_cell_length_b                   16.85390(10)
_cell_length_c                   15.73810(10)
_cell_measurement_reflns_used    55166
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.5817
_cell_measurement_theta_min      2.9817
_cell_volume                     3927.90(4)
_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, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -54.00  -27.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  125.0000  -90.0000 27

  2 omega  -42.00    8.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814   77.0000   90.0000 50

  3 omega    9.00   98.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -       41.0814 -125.0000 -120.0000 89

  4 omega   16.00  108.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -       41.0814   37.0000   30.0000 92

  5 omega   29.00   69.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   30.0000 40

  6 omega   38.00   65.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  150.0000 27

  7 omega   32.00   69.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  120.0000 37

  8 omega   40.00   68.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -60.0000 28

  9 omega   37.00   64.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -120.0000 27

 10 omega   84.00  113.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -90.0000 29

 11 omega  123.00  156.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -90.0000 33

 12 omega   84.00  114.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000  150.0000 30

 13 omega  127.00  156.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000  150.0000 29

 14 omega   41.00   95.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -61.0000 -180.0000 54

 15 omega  125.00  152.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -180.0000 27

 16 omega   53.00  123.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -61.0000 -120.0000 70

 17 omega   30.00   62.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   90.0000 32

 18 omega   29.00   69.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -90.0000 40

 19 omega   37.00   66.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -150.0000 29

 20 omega  -67.00   35.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814   37.0000 -150.0000 102

 21 omega  -98.00   -2.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  125.0000    0.0000 96

 22 omega   11.00  115.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -       41.0814   57.0000  -90.0000 104

 23 omega    7.00  120.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -       41.0814   77.0000   60.0000 113

 24 omega   11.00  115.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -       41.0814   57.0000  150.0000 104

 25 omega   76.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000   60.0000 82

 26 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -90.0000 85

 27 omega   32.00  121.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000   90.0000 89

 28 omega   76.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000  120.0000 82

 29 omega   23.00  109.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  150.0000 86

 30 omega   79.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -30.0000 79

 31 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  150.0000 85

 32 omega   23.00  109.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  -90.0000 86

 33 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000    0.0000 81

 34 omega   79.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -150.0000 79

 35 omega  -71.00   33.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814   57.0000  -60.0000 104

 36 omega -120.00   -7.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -77.0000 -180.0000 113

 37 omega -117.00  -15.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -37.0000 -180.0000 102

 38 omega    7.00  120.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -       41.0814   77.0000  -30.0000 113

 39 omega    7.00  120.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -       41.0814   77.0000 -180.0000 113

 40 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   60.0000 81

 41 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -30.0000 81

 42 omega   79.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -120.0000 79

 43 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   90.0000 85

 44 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   30.0000 81

 45 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  120.0000 85

 46 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -120.0000 81

 47 omega   32.00   77.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  120.0000 45

 48 omega   32.00  121.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  150.0000 89

 49 omega   28.00  141.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000  -30.0000 113

 50 omega -115.00  -11.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000  -90.0000 104

 51 omega -117.00  -15.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -37.0000   30.0000 102

 52 omega -120.00   -7.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -77.0000   90.0000 113

 53 omega -115.00  -11.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000    0.0000 104

 54 omega -115.00  -11.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000 -180.0000 104

 55 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -90.0000 81

 56 omega   74.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   74.0000    0.0000 84

 57 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -150.0000 81

 58 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -30.0000 85

 59 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   30.0000 85

 60 omega   29.00   69.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -30.0000 40

 61 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  150.0000 81

 62 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -60.0000 81

 63 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -180.0000 81

 64 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   60.0000 85

 65 omega -117.00  -15.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -37.0000  -30.0000 102

 66 omega -118.00   -8.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -74.0000 -128.0000 110

 67 omega -115.00  -11.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000   90.0000 104

 68 omega -117.00  -15.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -37.0000  -90.0000 102

 69 omega -115.00  -11.00   1.0000    1.3950
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000  -60.0000 104

 70 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   90.0000 81

 71 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -60.0000 85

 72 omega   77.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  120.0000 81

 73 omega   32.00  121.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  -90.0000 89

 74 omega   73.00  158.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -120.0000 85

 75 omega   73.00  155.00   1.0000   18.6600
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -150.0000 82
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0005883000
_diffrn_orient_matrix_UB_12      -0.0323005000
_diffrn_orient_matrix_UB_13      -0.0916691000
_diffrn_orient_matrix_UB_21      -0.0636586000
_diffrn_orient_matrix_UB_22      0.0677305000
_diffrn_orient_matrix_UB_23      -0.0354451000
_diffrn_orient_matrix_UB_31      0.0822422000
_diffrn_orient_matrix_UB_32      0.0522199000
_diffrn_orient_matrix_UB_33      -0.0106967000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            129446
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.736
_diffrn_reflns_theta_min         3.820
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.314
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.174
_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            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.2965
_exptl_crystal_size_mid          0.2452
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0458P)^2^+0.0344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7215
_reflns_number_total             7934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06883a2.cif
_cod_data_source_block           1
_cod_database_code               7125111
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Fe1 Co1 P6 F6 Si1 C31 H55'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              6998
_olex2_submission_special_instructions 'No special instructions were received'