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_7125109
_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 Fe2 N P5'
_chemical_formula_sum            'C29 H50 Fe2 N P5'
_chemical_formula_weight         679.25
_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                 114.972(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2557(3)
_cell_length_b                   12.4359(2)
_cell_length_c                   16.6796(3)
_cell_measurement_reflns_used    8171
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      32.3439
_cell_measurement_theta_min      2.8433
_cell_volume                     3244.67(11)
_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      122.99(10)
_diffrn_detector_area_resol_mean 15.9702
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details
;
  1 omega    1.00   91.00   0.2500  100.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0384   77.0000   60.0000 360

  2 omega   52.00   88.00   0.2500  100.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0384   57.0000 -180.0000 144

  3 omega  -43.00   45.00   0.2500  100.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0384  -57.0000  -60.0000 352

  4 omega    1.00   38.00   0.2500  100.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0384   38.0000  -30.0000 148
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0007143000
_diffrn_orient_matrix_UB_12      0.0549304000
_diffrn_orient_matrix_UB_13      -0.0113179000
_diffrn_orient_matrix_UB_21      0.0347903000
_diffrn_orient_matrix_UB_22      0.0108844000
_diffrn_orient_matrix_UB_23      0.0406386000
_diffrn_orient_matrix_UB_31      0.0314459000
_diffrn_orient_matrix_UB_32      -0.0108123000
_diffrn_orient_matrix_UB_33      -0.0166598000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20562
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.417
_diffrn_reflns_theta_min         2.849
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.914
_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    1.390
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.1021
_exptl_crystal_size_mid          0.0655
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         10520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0232P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6944
_reflns_number_total             10520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06883a2.cif
_cod_data_source_block           1abs
_cod_database_code               7125109
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C29 H50 Fe2 P5 N1'
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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:
 C14(H14), C11(H11)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C22(H22A,H22B,H22C), C25(H25A,H25B,
 H25C), C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C21(H21A,
 H21B,H21C), C29(H29A,H29B,H29C), C19(H19A,H19B,H19C), C28(H28A,H28B,H28C),
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C)
;
_shelx_res_checksum              27412
_olex2_submission_special_instructions 'No special instructions were received'