Transition-Metal Carbonyl Complexes of 2,5-Diferrocenyl-1-phenyl-1H-phosphole
Miesel, Dominique; Hildebrandt, Alexander; Korb, Marcus; Schaarschmidt, Dieter; Lang, Heinrich; Organometallics 34 (2015) 4293–; doi:10.1021/acs.organomet.5b00520

data_4087704
_publ_section_title
;
 Transition-Metal Carbonyl Complexes of
 2,5-Diferrocenyl-1-phenyl-1H-phosphole
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4293
_journal_paper_doi               10.1021/acs.organomet.5b00520
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C35 H25 Fe2 O5 P W'
_chemical_formula_sum            'C35 H25 Fe2 O5 P W'
_chemical_formula_weight         852.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.437(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5986(8)
_cell_length_b                   13.4025(7)
_cell_length_c                   18.1802(17)
_cell_measurement_reflns_used    5316
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      27.1030
_cell_measurement_theta_min      3.0460
_cell_volume                     3124.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      111(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13942
_diffrn_reflns_point_group_measured_fraction_full 0.654
_diffrn_reflns_point_group_measured_fraction_max 0.654
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.040
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.682
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.692
_refine_diff_density_min         -2.445
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details
;
 Flack x determined using 1158 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.228(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         7192
_refine_ls_number_restraints     830
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0342P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.310
_reflns_Friedel_fraction_full    0.310
_reflns_Friedel_fraction_max     0.310
_reflns_number_gt                5921
_reflns_number_total             7192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00520_si_001.cif
_cod_data_source_block           DM-PWX1
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4087704
_shelxl_version_number           2013-4
_shelx_res_checksum              91559
_shelx_hkl_checksum              43572