Syntheses, Structures, and Mössbauer Effect Spectroscopy of Triple-Decker Complexes Incorporating Nonamethylferrocene
Schwartz, Andrew J.; Pike, Robert D.; Herber, Rolfe H.; Watson, Eric J.; Organometallics 35 (2015) 62–; doi:10.1021/acs.organomet.5b00913

data_4088186
_publ_section_title
;
 Syntheses, Structures, and M\"ossbauer Effect Spectroscopy of
 Triple-Decker Complexes Incorporating Nonamethylferrocene
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              62
_journal_paper_doi               10.1021/acs.organomet.5b00913
_journal_volume                  35
_journal_year                    2015
_chemical_formula_moiety         'C29 H43 Fe2, P F6'
_chemical_formula_sum            'C29 H43 F6 Fe2 P'
_chemical_formula_weight         648.30
_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_method           SHELXL-2014/5
_cell_angle_alpha                90
_cell_angle_beta                 94.230(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7699(7)
_cell_length_b                   17.3782(14)
_cell_length_c                   19.3542(14)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.85
_cell_measurement_theta_min      3.42
_cell_volume                     2941.6(4)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2004)'
_computing_data_reduction        SAINTPLUS
_computing_molecular_graphics    'SHELXLE (Hubschle, 2011)'
_computing_publication_material  'Mercury 3.6 (CCDC, 2015)'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\w and \y'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34171
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         66.982
_diffrn_reflns_theta_min         3.422
_exptl_absorpt_coefficient_mu    8.907
_exptl_absorpt_correction_T_max  0.6099
_exptl_absorpt_correction_T_min  0.1452
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     630
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0559P)^2^+5.0474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4631
_reflns_number_total             5229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00913_si_001.cif
_cod_data_source_block           Watson029_0m_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088186
_shelx_estimated_absorpt_t_min   0.138
_shelx_estimated_absorpt_t_max   0.441
_shelxl_version_number           2014/5
_shelx_res_checksum              21612
_shelx_hkl_checksum              95444