#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:04:03 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180058 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/04/7050414.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050414
loop_
_publ_author_name
'Braunstein, Pierre'
'Clerc, Guislaine'
'Morise, Xavier'
_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         'C73 H70 B2 Cl6 Cu2 F8 Fe2 N4 O10 P4'
_chemical_formula_sum            'C73 H70 B2 Cl6 Cu2 F8 Fe2 N4 O10 P4'
_chemical_formula_weight         1912.39
_chemical_name_common            'Compound 2 1.5 CH2Cl2'
_chemical_name_systematic        ' ?'
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 111.598(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.4623(7)
_cell_length_b                   14.3872(6)
_cell_length_c                   12.4708(4)
_cell_measurement_reflns_used    13114
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      1.4
_cell_volume                     4080.9(3)
_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
;
13114 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  29. mm.
Scan angle =  2.0 deg 1 scans of   71 sec per frame.
Data collection was divided into  1 sets
with the following starting angles and number of frames :

Set 1 Theta =    8.85 Omega =  180.00 Kappa =    0.00   76 frames
Friedel pairs were not averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13114
_diffrn_reflns_theta_max         32.51
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.56
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.254
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.066
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.062
_refine_ls_wR_factor_ref         0.057
_reflns_number_gt                4571
_reflns_number_total             6229
_reflns_threshold_expression     >3.0σ(I)
_cod_data_source_file            b206410n.txt
_cod_data_source_block           st341
_cod_database_code               7050414
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,+y,-z
-x,-y,-z
+x,-y,+z
1/2+x,1/2+y,+z
1/2-x,1/2+y,-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
FE 0.88136(2) 0.0000 0.11455(4) 0.0236(2) 0.500 Uani ? ? Fe
CU 0.85943(2) 0.0000 0.29876(4) 0.0373(2) 0.500 Uani ? ? Cu
C1 0.9428(2) 0.0000 0.2492(3) 0.033(1) 0.500 Uani ? ? C
O1 0.9854(1) 0.0000 0.3307(3) 0.046(2) 0.500 Uani ? ? O
C2 0.8044(2) 0.0000 0.0842(3) 0.029(1) 0.500 Uani ? ? C
O2 0.7538(1) 0.0000 0.0615(2) 0.037(1) 0.500 Uani ? ? O
C3 0.9092(1) 0.0000 0.0007(3) 0.027(1) 0.500 Uani ? ? C
O3 0.9279(1) 0.0000 -0.0708(2) 0.040(1) 0.500 Uani ? ? O
P1 0.87618(2) 0.15476(4) 0.10841(5) 0.0240(2) 1.000 Uani ? ? P
C4 0.9452(1) 0.2183(2) 0.1694(2) 0.0261(9) 1.000 Uani ? ? C
C5 0.9510(1) 0.3004(2) 0.2315(2) 0.035(1) 1.000 Uani ? ? C
C6 1.0039(1) 0.3493(2) 0.2692(2) 0.038(1) 1.000 Uani ? ? C
C7 1.0510(1) 0.3170(2) 0.2446(2) 0.038(1) 1.000 Uani ? ? C
C8 1.0462(1) 0.2349(2) 0.1850(2) 0.042(1) 1.000 Uani ? ? C
C9 0.9939(1) 0.1851(2) 0.1483(2) 0.035(1) 1.000 Uani ? ? C
C10 0.8423(1) 0.2052(2) -0.0364(2) 0.0270(9) 1.000 Uani ? ? C
C11 0.8457(1) 0.3009(2) -0.0527(2) 0.031(1) 1.000 Uani ? ? C
C12 0.8217(1) 0.3393(2) -0.1620(2) 0.034(1) 1.000 Uani ? ? C
C13 0.7944(1) 0.2829(2) -0.2564(2) 0.034(1) 1.000 Uani ? ? C
C14 0.7902(1) 0.1887(2) -0.2419(2) 0.033(1) 1.000 Uani ? ? C
C15 0.8135(1) 0.1494(2) -0.1318(2) 0.030(1) 1.000 Uani ? ? C
C16 0.8286(1) 0.2100(2) 0.1759(2) 0.0269(9) 1.000 Uani ? ? C
C17 0.8472(1) 0.1988(2) 0.3033(2) 0.0295(9) 1.000 Uani ? ? C
O4 0.85073(9) 0.2781(1) 0.3622(1) 0.0383(9) 1.000 Uani ? ? O
C18 0.8709(2) 0.2521(2) 0.4833(3) 0.053(2) 1.000 Uani ? ? C
C19 0.8711(1) 0.1470(2) 0.4830(2) 0.044(1) 1.000 Uani ? ? C
N 0.8582(1) 0.1235(2) 0.3603(2) 0.0355(9) 1.000 Uani ? ? N
B 0.7858(2) 0.5000 0.5649(4) 0.041(2) 0.500 Uani ? ? B
F1 0.8454(2) 0.5000 0.6302(4) 0.088(2) 0.500 Uani ? ? F
F2 0.7559(1) 0.5000 0.6387(2) 0.058(1) 0.500 Uani ? ? F
F3 0.7737(1) 0.4211(2) 0.4991(2) 0.076(1) 1.000 Uani ? ? F
C20 0.8488(2) 0.5000 0.3529(3) 0.041(2) 0.500 Uani ? ? C
CL2 0.92568(5) 0.5000 0.4264(1) 0.0555(6) 0.500 Uani ? ? Cl
CL1 0.83088(6) 0.5000 0.2011(1) 0.0533(6) 0.500 Uani ? ? Cl
CL3 0.94173(9) 0.5000 0.0052(3) 0.110(2) 0.500 Uani ? ? Cl
C21 1.0000 0.543(1) 0.0000 0.132(9) 0.250 Uani ? ? C
H1 0.9186 0.3232 0.2484 0.0456 1.000 Uiso calc C5 H
H2 1.0074 0.4051 0.3120 0.0509 1.000 Uiso calc C6 H
H3 1.0867 0.3512 0.2688 0.0508 1.000 Uiso calc C7 H
H4 1.0788 0.2122 0.1689 0.0550 1.000 Uiso calc C8 H
H5 0.9912 0.1279 0.1085 0.0453 1.000 Uiso calc C9 H
H6 0.8646 0.3399 0.0118 0.0406 1.000 Uiso calc C11 H
H7 0.8240 0.4044 -0.1721 0.0445 1.000 Uiso calc C12 H
H8 0.7786 0.3092 -0.3314 0.0441 1.000 Uiso calc C13 H
H9 0.7714 0.1502 -0.3069 0.0434 1.000 Uiso calc C14 H
H10 0.8098 0.0846 -0.1220 0.0388 1.000 Uiso calc C15 H
H11 0.7904 0.1842 0.1413 0.0348 1.000 Uiso calc C16 H
H12 0.8272 0.2747 0.1597 0.0348 1.000 Uiso calc C16 H
H13 0.8449 0.2751 0.5178 0.0793 1.000 Uiso calc C18 H
H14 0.9094 0.2754 0.5237 0.0793 1.000 Uiso calc C18 H
H15 0.8415 0.1232 0.5079 0.0595 1.000 Uiso calc C19 H
H16 0.9083 0.1235 0.5310 0.0595 1.000 Uiso calc C19 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.001 International_Tables_Vol_IV_Table_2.3.1
B ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Cu ? 0.263 1.266 International_Tables_Vol_IV_Table_2.3.1
F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1
Fe ? 0.301 0.845 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1
P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CU FE C1 62.4(1) . . . ?
CU FE C2 68.5(1) . . . ?
CU FE C3 170.5(1) . . . ?
CU FE P1 90.16(2) . . . ?
CU FE P1 90.16(2) . . 4_555 ?
C1 FE C2 131.0(2) . . . ?
C1 FE C3 108.1(2) . . . ?
C1 FE P1 92.84(2) . . . ?
C1 FE P1 92.84(2) . . 4_555 ?
C2 FE C3 121.0(2) . . . ?
C2 FE P1 87.16(2) . . . ?
C2 FE P1 87.16(2) . . 4_555 ?
C3 FE P1 90.36(2) . . . ?
C3 FE P1 90.36(2) . . 4_555 ?
P1 FE P1 173.75(4) . . 4_555 ?
FE CU C1 42.9(1) . . . ?
FE CU C2 41.14(9) . . . ?
FE CU N 113.33(7) . . . ?
FE CU N 113.33(7) . . 4_555 ?
C1 CU C2 84.0(1) . . . ?
C1 CU N 104.25(8) . . . ?
C1 CU N 104.25(8) . . 4_555 ?
C2 CU N 109.94(7) . . . ?
C2 CU N 109.94(7) . . 4_555 ?
N CU N 132.7(1) . . 4_555 ?
C4 P1 C10 103.0(1) . . . ?
C4 P1 C16 103.7(1) . . . ?
C10 P1 C16 98.4(1) . . . ?
P1 C4 C5 123.2(2) . . . ?
P1 C4 C9 118.3(2) . . . ?
C5 C4 C9 118.5(2) . . . ?
C4 C5 C6 120.6(2) . . . ?
C5 C6 C7 120.2(3) . . . ?
C6 C7 C8 119.8(3) . . . ?
C7 C8 C9 120.4(3) . . . ?
C4 C9 C8 120.5(3) . . . ?
P1 C10 C11 120.2(2) . . . ?
P1 C10 C15 121.1(2) . . . ?
C11 C10 C15 118.8(2) . . . ?
C10 C11 C12 120.6(2) . . . ?
C11 C12 C13 120.1(2) . . . ?
C12 C13 C14 120.1(2) . . . ?
C13 C14 C15 120.2(3) . . . ?
C10 C15 C14 120.1(2) . . . ?
P1 C16 C17 116.3(2) . . . ?
C16 C17 O4 115.1(2) . . . ?
C16 C17 N 127.4(2) . . . ?
O4 C17 N 117.5(2) . . . ?
C17 O4 C18 106.1(2) . . . ?
O4 C18 C19 104.8(2) . . . ?
C18 C19 N 103.4(2) . . . ?
C17 N C19 107.6(2) . . . ?
F1 B F2 108.2(4) . . . ?
F1 B F3 107.6(3) . . . ?
F1 B F3 107.6(3) . . 4_565 ?
F2 B F3 110.6(3) . . . ?
F2 B F3 110.6(3) . . 4_565 ?
F3 B F3 112.2(4) . . 4_565 ?
CL2 C20 CL1 110.6(2) . . . ?
C21 CL3 C21 46.0(9) . . 3_765 ?
CL3 C21 CL3 134.0(9) . . 3_765 ?
CL3 C21 C21 67.0(5) . . 3_765 ?
CL3 C21 C21 67.0(5) . 3_765 3_765 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
FE CU 2.5441(7) . . ?
FE CU 2.5441(7) . 4_555 ?
FE C1 1.795(4) . . ?
FE C1 1.795(4) . 4_555 ?
FE C2 1.777(4) . . ?
FE C2 1.777(4) . 4_555 ?
FE C3 1.786(4) . . ?
FE C3 1.786(4) . 4_555 ?
FE P1 2.2298(6) . . ?
FE P1 2.2298(6) . 4_555 ?
CU C1 2.339(4) . . ?
CU C1 2.339(4) . 4_555 ?
CU C2 2.514(4) . . ?
CU C2 2.514(4) . 4_555 ?
CU N 1.939(2) . . ?
CU N 1.939(2) . 4_555 ?
C1 O1 1.157(5) . . ?
C1 O1 1.157(5) . 4_555 ?
C2 O2 1.164(5) . . ?
C2 O2 1.164(5) . 4_555 ?
C3 O3 1.142(4) . . ?
C3 O3 1.142(4) . 4_555 ?
P1 C4 1.822(3) . . ?
P1 C10 1.837(2) . . ?
P1 C16 1.848(2) . . ?
C4 C5 1.391(4) . . ?
C4 C9 1.394(4) . . ?
C5 C6 1.393(4) . . ?
C6 C7 1.379(4) . . ?
C7 C8 1.377(4) . . ?
C8 C9 1.390(4) . . ?
C10 C11 1.399(3) . . ?
C10 C15 1.392(4) . . ?
C11 C12 1.384(4) . . ?
C12 C13 1.382(4) . . ?
C13 C14 1.377(4) . . ?
C14 C15 1.397(4) . . ?
C16 C17 1.491(3) . . ?
C17 O4 1.342(3) . . ?
C17 N 1.270(3) . . ?
O4 C18 1.455(4) . . ?
C18 C19 1.511(5) . . ?
C19 N 1.483(3) . . ?
B F1 1.382(7) . . ?
B F1 1.382(7) . 4_565 ?
B F2 1.371(6) . . ?
B F2 1.371(6) . 4_565 ?
B F3 1.367(3) . . ?
B F3 1.367(3) . 4_565 ?
C20 CL2 1.762(5) . . ?
C20 CL2 1.762(5) . 4_565 ?
C20 CL1 1.779(5) . . ?
C20 CL1 1.779(5) . 4_565 ?
CL3 C21 1.576(6) . . ?
CL3 C21 1.576(6) . 3_765 ?
CL3 C21 1.576(6) . 2_755 ?
CL3 C21 1.576(6) . 4_565 ?
C21 C21 1.23(3) . 3_765 ?
C21 C21 1.23(3) . 4_565 ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
