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_4087691
_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            'C36 H39 Fe P Ru2'
_chemical_formula_weight         760.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                84.99(2)
_cell_angle_beta                 84.428(15)
_cell_angle_gamma                74.283(10)
_cell_formula_units_Z            2
_cell_length_a                   11.188(2)
_cell_length_b                   11.744(4)
_cell_length_c                   11.936(4)
_cell_measurement_reflns_used    9420
_cell_measurement_temperature    110
_cell_measurement_theta_max      39.83
_cell_measurement_theta_min      3.43
_cell_volume                     1499.5(8)
_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-2014
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.983
_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_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48657
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         43.703
_diffrn_reflns_theta_min         2.665
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.550
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       Prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.448
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         22682
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15219
_reflns_number_total             22682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00496_si_007.cif
_cod_data_source_block           12
_cod_original_cell_volume        1499.4(8)
_cod_database_code               4087691
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.682
_shelx_estimated_absorpt_t_max   0.893
_shelx_res_checksum              31963
_shelx_hkl_checksum              93243