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_7125108
_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 Fe N Ni P5'
_chemical_formula_sum            'C29 H50 Fe N Ni P5'
_chemical_formula_weight         682.11
_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             2015-02-11
_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                 107.7100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.74830(10)
_cell_length_b                   15.47460(10)
_cell_length_c                   17.3699(2)
_cell_measurement_reflns_used    8240
_cell_measurement_temperature    123.1(8)
_cell_measurement_theta_max      66.2719
_cell_measurement_theta_min      3.6364
_cell_volume                     3264.25(5)
_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      123.1(8)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega   29.00  116.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   38.0000  120.0000 174

  2 omega  -33.00   37.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431  -38.0000  -30.0000 140

  3 omega   20.00   77.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 114

  4 omega   35.00   96.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   90.0000 122

  5 omega   77.00  164.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -90.0000 174

  6 omega   31.00   66.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -120.0000 70

  7 omega   25.00  122.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  120.0000 194

  8 omega    8.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   77.0000 -150.0000 224

  9 omega   12.00  115.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   57.0000    0.0000 206

 10 omega   63.00  165.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000   60.0000 204
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0600469000
_diffrn_orient_matrix_UB_12      0.0416073000
_diffrn_orient_matrix_UB_13      0.0821242000
_diffrn_orient_matrix_UB_21      0.1083276000
_diffrn_orient_matrix_UB_22      -0.0000487000
_diffrn_orient_matrix_UB_23      -0.0220014000
_diffrn_orient_matrix_UB_31      -0.0274609000
_diffrn_orient_matrix_UB_32      0.0904178000
_diffrn_orient_matrix_UB_33      -0.0378583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15331
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.388
_diffrn_reflns_theta_min         3.804
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.736
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.434
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.1888
_exptl_crystal_size_mid          0.1649
_exptl_crystal_size_min          0.0639
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4600
_reflns_number_total             5591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06883a2.cif
_cod_data_source_block           1
_cod_database_code               7125108
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C29H50FeNiP5N
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.30
_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:
 C2(H2), C5(H5)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C)
;
_shelx_res_checksum              32302
_olex2_submission_special_instructions 'No special instructions were received'