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_7125110
_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 Cr Fe P5 Si'
_chemical_formula_sum            'C31 H55 Cr Fe P5 Si'
_chemical_formula_weight         718.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-11
_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                 106.4910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9256(2)
_cell_length_b                   11.62750(10)
_cell_length_c                   16.4157(2)
_cell_measurement_reflns_used    34983
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.1925
_cell_measurement_theta_min      3.0870
_cell_volume                     3646.82(7)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega   15.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   37.0000  -90.0000 99

  2 omega   67.00  113.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   57.0000  120.0000 46

  3 omega   49.00  118.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814  161.0000 -124.0000 69

  4 omega   12.00   38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   57.0000  120.0000 26

  5 omega  -77.00  -51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   45.0000   60.0000 26

  6 omega   34.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -45.0000   90.0000 41

  7 omega   63.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -94.0000 -180.0000 40

  8 omega   30.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -94.0000   60.0000 63

  9 omega   33.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -30.0000 -150.0000 33

 10 omega   34.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -61.0000  -90.0000 94

 11 omega   39.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -45.0000  150.0000 29

 12 omega   33.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -94.0000  120.0000 63

 13 omega   47.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   15.0000 -120.0000 111

 14 omega    7.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   77.0000  150.0000 113

 15 omega  -38.00   75.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814  -77.0000  -90.0000 113

 16 omega   11.00  115.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   57.0000    0.0000 104

 17 omega   78.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   30.0000  120.0000 80

 18 omega   78.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   30.0000  -60.0000 80

 19 omega   30.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -30.0000   30.0000 39

 20 omega   24.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -94.0000 -120.0000 85

 21 omega   30.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -30.0000  120.0000 39

 22 omega   47.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   15.0000   60.0000 111

 23 omega  -98.00   -2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  125.0000  120.0000 96

 24 omega    2.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814 -125.0000   90.0000 96

 25 omega    7.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   77.0000   30.0000 113

 26 omega -162.00  -49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  -30.0000 113

 27 omega -162.00  -49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000 -180.0000 113

 28 omega -162.00  -49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000   60.0000 113

 29 omega -161.00  -50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -76.0000 -114.3784 111

 30 omega   75.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   77.0000  120.0000 83

 31 omega   33.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300 -125.0000   60.0000 89

 32 omega -115.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000   60.0000 104

 33 omega    7.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   77.0000  -30.0000 113

 34 omega    7.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   77.0000 -120.0000 113

 35 omega -162.00  -49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  -69.7934 113

 36 omega -160.00  -50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -74.0000    9.7741 110

 37 omega -162.00  -96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  120.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0087467000
_diffrn_orient_matrix_UB_12      0.0817477000
_diffrn_orient_matrix_UB_13      -0.0624848000
_diffrn_orient_matrix_UB_21      -0.0538756000
_diffrn_orient_matrix_UB_22      -0.0907119000
_diffrn_orient_matrix_UB_23      -0.0495624000
_diffrn_orient_matrix_UB_31      -0.0812469000
_diffrn_orient_matrix_UB_32      0.0513621000
_diffrn_orient_matrix_UB_33      0.0119776000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63463
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.354
_diffrn_reflns_theta_min         4.451
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.171
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.422
_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 green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.1546
_exptl_crystal_size_mid          0.1162
_exptl_crystal_size_min          0.0639
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0497P)^2^+0.5116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6576
_reflns_number_total             7334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06883a2.cif
_cod_data_source_block           1
_cod_database_code               7125110
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C31H55FeCrSiP5
_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:
 C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C18(H18A,H18B,
 H18C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C7(H7A,
 H7B,H7C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C8(H8A,H8B,H8C), C6(H6A,
 H6B,H6C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              39614
_olex2_submission_special_instructions 'No special instructions were received'