Cyclopropanation and Diels‒Alder reactions catalyzed by the first heterobimetallic complexes with bridging phosphinooxazoline ligands
Braunstein, Pierre; Clerc, Guislaine; Morise, Xavier; New Journal of Chemistry 27 (2003) 68–72; doi:10.1039/b206410n

data_7050413
_publ_section_title
;
 Cyclopropanation and Diels--Alder reactions catalyzed by the first
 heterobimetallic complexes with bridging phosphinooxazoline ligands
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              68
_journal_page_last               72
_journal_paper_doi               10.1039/b206410n
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         'C35 H32 Fe N2 O5 P2'
_chemical_formula_sum            'C35 H32 Fe N2 O5 P2'
_chemical_formula_weight         678.45
_chemical_name_systematic        ?
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   41.966(1)
_cell_length_b                   34.575(1)
_cell_length_c                   9.741(1)
_cell_measurement_reflns_used    17857
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     14133.9(15)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
17857 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  2.0 deg 1 scans of   60 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    8.50 Omega =  180.00 Kappa =    0.00   77 frames
Set 2 Theta =   -6.70 Kappa = -132.00 Phi   =    0.00   13 frames
Friedel pairs were not averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            17857
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.28
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             5632
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.051
_refine_ls_abs_structure_details 'Flack H D  (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.802
_refine_ls_goodness_of_fit_ref   1.361
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     441
_refine_ls_number_reflns         2614
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.022
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.106
_refine_ls_wR_factor_ref         0.079
_reflns_number_gt                2614
_reflns_number_total             4422
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b206410n.txt
_cod_data_source_block           st499
_cod_original_cell_volume        14133(2)
_cod_original_sg_symbol_Hall     ' F 2 -2d'
_cod_database_code               7050413