Synthesis of the Bifunctional Phosphinidene Cluster, Fe3(CO)9(μ3-PH)2, and a Systematic Study of the Reactivity of the Cluster-Bound P-H Functional Group
Caryn C. Borg-Breen; Maria T. Bautista; Cynthia K. Schauer; Peter S. White; Journal of the American Chemical Society 122 (2000) 3952–3962; doi:10.1021/ja993811f

data_4115976
_publ_section_title
;
 Synthesis of the Bifunctional Phosphinidene Cluster, Fe3(CO)9(\m3-PH)2,
 and a Systematic Study of the Reactivity of the Cluster-Bound P-H
 Functional Group
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3952
_journal_page_last               3962
_journal_paper_doi               10.1021/ja993811f
_journal_volume                  122
_journal_year                    2000
_chemical_formula_moiety         'C15 H8 Fe3 N2 O9 P2'
_chemical_formula_sum            'C15 H8 Fe3 N2 O9 P2'
_chemical_formula_weight         589.72
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 99.906(1)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.7382(5)
_cell_length_b                   9.7384(4)
_cell_length_c                   18.6132(8)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    193
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.50
_cell_volume                     2095.98(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT/NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      193
_diffrn_measurement_device       'Bruker SMART 1K  '
_diffrn_measurement_method       'Omega scan    '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23774
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    2.25
_exptl_absorpt_correction_T_max  1.279
_exptl_absorpt_correction_T_min  .806
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_F_000             1173.77
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.28
_refine_ls_extinction_coef       0.429(193)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_obs   2.66
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5615
_refine_ls_R_factor_all          0.027
_refine_ls_R_factor_obs          0.023
_refine_ls_shift/esd_max         0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.030
_refine_ls_wR_factor_obs         0.029
_reflns_number_observed          5623
_reflns_number_total             6048
_reflns_observed_criterion       'Inet > 3.0\s(Inet)'
_cod_data_source_file            ja993811f_1.cif
_cod_data_source_block           c98003
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/\s^2^(F)' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w = 1/\s^2^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4115976