Synthesis and Characterization of a Family of Air-Stable Ferrocene- and Ruthenocene-Containing Primary, Secondary, and Tertiary Phosphines
Kenaree, Amir Rabiee; Cuthbert, Tyler J.; Barbon, Stephanie M.; Boyle, Paul D.; Gillies, Elizabeth R.; Ragogna, Paul J.; Gilroy, Joe B.; Organometallics 34 (2015) 4272–; doi:10.1021/acs.organomet.5b00496

data_4087687
_publ_section_title
;
 Synthesis and Characterization of a Family of Air-Stable Ferrocene- and
 Ruthenocene-Containing Primary, Secondary, and Tertiary Phosphines
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4272
_journal_paper_doi               10.1021/acs.organomet.5b00496
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C24 H27 P Ru2'
_chemical_formula_weight         548.56
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.331(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.614(4)
_cell_length_b                   5.7191(7)
_cell_length_c                   25.299(3)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    110
_cell_measurement_theta_max      34.48
_cell_measurement_theta_min      3.24
_cell_volume                     4067.3(9)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10181
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.304
_diffrn_reflns_theta_min         3.706
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  0.438262
_exptl_absorpt_correction_T_min  0.33943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.585
_refine_diff_density_min         -1.680
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         10181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0346P)^2^+31.9336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9458
_reflns_number_total             10181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00496_si_007.cif
_cod_data_source_block           8b
_cod_original_cell_volume        4067.4(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4087687
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.609
_shelx_estimated_absorpt_t_max   0.909
_exptl_absorpt_special_details
; 
Sample crystal was non-merohedrally twinned by an approximate 180 degree rotation about the [1,-1,-1].  The twin fraction parameter refined to a value of 0.41202(74).
;
_shelx_res_checksum              76376
_shelx_hkl_checksum              13639