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_4130416
_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 Fe O3 P2, 2(C9 H12)'
_chemical_formula_sum            'C51 H78 Fe O3 P2'
_chemical_formula_weight         856.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 106.467(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0820(3)
_cell_length_b                   23.0562(9)
_cell_length_c                   17.1097(6)
_cell_measurement_temperature    173(2)
_cell_volume                     4949.0(3)
_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 0.975
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8529
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.051
_diffrn_reflns_theta_min         2.159
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.9414
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Scalepack
_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    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_recrystallization_method 'crystallized from DCM/Hexane/Benzene'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0402P)^2^+0.9720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3232
_reflns_number_total             4369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03178_si_002.cif
_cod_data_source_block           lw02
_cod_database_code               4130416
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.941
_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:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C25(H25), C35(H35), C52(H52), C54(H54), C56(H56)
2.c Idealised Me refined as rotating group:
 C51A(H51A,H51B,H51C), C53A(H53A,H53B,H53C), C55A(H55A,H55B,H55C)
;
_shelx_res_checksum              62976
_shelx_hkl_checksum              24355
_olex2_date_sample_data_collection 1097791200
_olex2_date_sample_submission    1097100000
_olex2_exptl_crystal_mounting_method 'mounted on a glas fibre'
_olex2_submission_special_instructions 'No special instructions were received'