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_4087688
_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            'C19 H20.5 Cl3 P0.5 Ru1.5'
_chemical_formula_weight         522.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90
_cell_angle_beta                 100.311(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.778(3)
_cell_length_b                   27.701(19)
_cell_length_c                   12.417(9)
_cell_measurement_reflns_used    8712
_cell_measurement_temperature    110
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.77
_cell_volume                     1955(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0625
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35309
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.416
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 2654 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7915
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0389P)^2^+0.8685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                6525
_reflns_number_total             7915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00496_si_007.cif
_cod_data_source_block           8c
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C19 H20.50 Cl3 P0.50 Ru1.50'
_cod_database_code               4087688
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.724
_shelx_estimated_absorpt_t_max   0.925
_shelx_res_checksum              49334
_shelx_hkl_checksum              39735