An efficient, scalable synthesis of ferrocenylphosphine and dichloroferrocenylphosphine
Surgenor, Brian; Taylor, Laurence J.; Nordheider, Andreas; Slawin, Alexandra; Arachchige, Kasun; Woollins, J. D.; Kilian, Petr; RSC Adv.  (2016) –; doi:10.1039/C5RA27594F

data_7223820
_publ_section_title
;
 An efficient, scalable synthesis of ferrocenylphosphine and
 dichloroferrocenylphosphine
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA27594F
_journal_year                    2016
_chemical_formula_moiety         'C10 H11 Fe P'
_chemical_formula_sum            'C10 H11 Fe P'
_chemical_formula_weight         218.02
_chemical_name_common            FcPH2
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-12
_audit_creation_method           'by CrystalStructure 4.1'
_audit_update_record
;
2015-11-16 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 112.071(18)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.658(10)
_cell_length_b                   7.528(5)
_cell_length_c                   10.432(8)
_cell_measurement_reflns_used    2704
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.74
_cell_volume                     921.2(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5398
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.299
_diffrn_reflns_theta_min         1.736
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             448.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.68
_refine_diff_density_min         -1.64
_refine_ls_extinction_coef       0.008(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1662
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1408P)^2^+3.4699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2450
_refine_ls_wR_factor_ref         0.2629
_reflns_number_gt                1285
_reflns_number_total             1662
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5ra27594f2.cif
_cod_data_source_block           FcPH2
_cod_database_code               7223820
_shelx_res_checksum              74494