Gyroscope-Like Complexes Based on Dibridgehead Diphosphine Cages That Are Accessed by Three-Fold Intramolecular Ring Closing Metatheses and Encase Fe(CO)3, Fe(CO)2(NO)(+), and Fe(CO)3(H)(+) Rotators.
Lang, Georgette M.; Shima, Takanori; Wang, Leyong; Cluff, Kyle J.; Skopek, Katrin; Hampel, Frank; Blümel, Janet; Gladysz, John A.; Journal of the American Chemical Society 138 (2016) 7649–7663; doi:10.1021/jacs.6b03178

data_4130415
_publ_section_title
;
 Gyroscope-Like Complexes Based on Dibridgehead Diphosphine Cages That Are
 Accessed by Three-Fold Intramolecular Ring Closing Metatheses and Encase
 Fe(CO)3, Fe(CO)2(NO)(+), and Fe(CO)3(H)(+) Rotators.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7649
_journal_page_last               7663
_journal_paper_doi               10.1021/jacs.6b03178
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C33 H54 Fe1 O3 P2, C6 H6'
_chemical_formula_sum            'C39 H60 Fe O3 P2'
_chemical_formula_weight         694.66
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.835(2)
_cell_length_b                   15.835(2)
_cell_length_c                   27.470(6)
_cell_measurement_temperature    173(2)
_cell_volume                     5965.2(17)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.860
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.860
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            3060
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         2.573
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.8597
_exptl_absorpt_correction_T_min  0.8113
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             2244
_exptl_crystal_recrystallization_method 'crystallized from DCM/Hexane/Benzene'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00039(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+17.3775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                918
_reflns_number_total             1337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03178_si_002.cif
_cod_data_source_block           lw01_2
_cod_original_cell_volume        5965(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4130415
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C100(H100), C15(H15)
;
_shelx_res_checksum              11078
_shelx_hkl_checksum              82246
_olex2_date_sample_data_collection 1092693600
_olex2_date_sample_submission    1092348000
_olex2_exptl_crystal_mounting_method 'mounted on a glas fibre'
_olex2_submission_special_instructions 'No special instructions were received'