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_7125107
_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         'C29 H50 Co Fe N P5'
_chemical_formula_sum            'C29 H50 Co Fe N P5'
_chemical_formula_weight         682.33
_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             2015-02-10
_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                 108.2580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.73000(10)
_cell_length_b                   15.57900(10)
_cell_length_c                   17.30440(10)
_cell_measurement_reflns_used    9010
_cell_measurement_temperature    123.1(6)
_cell_measurement_theta_max      66.4674
_cell_measurement_theta_min      3.6532
_cell_volume                     3259.05(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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
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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      123.1(6)
_diffrn_detector_area_resol_mean 5.2715
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -32.00   69.00   0.5000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431  -57.0000 -120.0000 202

  2 omega    7.00   92.00   0.5000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431 -125.0000  120.0000 170

  3 omega  126.00  165.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000   90.0000 78

  4 omega   27.00   60.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 66

  5 omega   11.00   82.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   30.0000 142

  6 omega   41.00  120.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -120.0000 158

  7 omega   61.00  107.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  120.0000 92

  8 omega  127.00  154.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000    0.0000 54

  9 omega  135.00  168.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  120.0000 66

 10 omega   32.00   60.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -30.0000 56

 11 omega  143.00  175.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -120.0000 64

 12 omega   22.00   68.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  150.0000 92

 13 omega   33.00   84.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -180.0000 102

 14 omega   75.00  118.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000    0.0000 86

 15 omega   28.00   65.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   90.0000 74

 16 omega   63.00  115.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000   90.0000 104

 17 omega -120.00  -80.00   0.5000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4431  -77.0000    0.0000 80
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0211753000
_diffrn_orient_matrix_UB_12      -0.0651376000
_diffrn_orient_matrix_UB_13      0.0604675000
_diffrn_orient_matrix_UB_21      0.1149625000
_diffrn_orient_matrix_UB_22      -0.0396917000
_diffrn_orient_matrix_UB_23      0.0125852000
_diffrn_orient_matrix_UB_31      0.0506790000
_diffrn_orient_matrix_UB_32      0.0629319000
_diffrn_orient_matrix_UB_33      0.0705444000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17145
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         66.572
_diffrn_reflns_theta_min         3.800
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.017
_exptl_absorpt_correction_T_max  0.555
_exptl_absorpt_correction_T_min  0.463
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.1206
_exptl_crystal_size_mid          0.0983
_exptl_crystal_size_min          0.0882
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0444P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4810
_reflns_number_total             5732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06883a2.cif
_cod_data_source_block           1
_cod_database_code               7125107
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C29 H50 Fe Co P5 N'
_reflns_odcompleteness_completeness 98.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              14363
_olex2_submission_special_instructions 'No special instructions were received'