1,3-Dipolar Cycloaddition to the Fe−OC Fragment. 19. Synthesis and Properties of Fe(CO)2(PR3)(R1NC(R2)−C(R3)O) and Fe(CO)(Ph2PCH2CH2PPh2)(R1NC(R2)−C(R3)O) and Their Reactivity toward Dipolarophiles. First X-ray Crystal Structure of the Initial Bicyclo[2.2.1] Adduct
Siebenlist, Ron; Frühauf, Hans-Werner; Vrieze, Kees; Smeets, Wilberth J. J.; Spek, Anthony L.; Organometallics 21 (2002) 5628–; doi:10.1021/om020605z

data_4077115
_publ_section_title
;
 1,3-Dipolar Cycloaddition to the Fe&#x2212;OC Fragment. 19. Synthesis and
 Properties of Fe(CO)2(PR3)(R1NC(R2)&#x2212;C(R3)O) and
 Fe(CO)(Ph2PCH2CH2PPh2)(R1NC(R2)&#x2212;C(R3)O) and Their Reactivity
 toward Dipolarophiles. First X-ray Crystal Structure of the Initial
 Bicyclo[2.2.1] Adduct
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5628
_journal_paper_doi               10.1021/om020605z
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C45 H45 Fe N O6 P2'
_chemical_formula_sum            'C45 H45 Fe N O6 P2'
_chemical_formula_weight         813.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 125.762(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5238(7)
_cell_length_b                   23.0239(15)
_cell_length_c                   18.7570(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     4038.3(5)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection
'Locally modified CAD4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Turbo-CAD4
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.1501
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7395
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7114
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                3857
_reflns_number_total             7114
_reflns_threshold_expression     I>2\\s(I)
_cod_data_source_file            om020605z.cif
_cod_data_source_block           s1223a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_sites_solution_hydrogens' value 'geom ' changed
to 'geom' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_sites_solution_primary' value 'direct ' changed
to 'direct' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_sites_solution_secondary' value 'difmap ' changed
to 'difmap' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'noref ' changed
to 'noref' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_weighting_scheme' value 'calc ' changed to
'calc' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4077115