#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:11:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230405 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/74/7057479.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_7057479
loop_
_publ_author_name
'Bárta, Ondřej'
'Drusan, Michal'
'Císařová, Ivana'
'Šebesta, Radovan'
'Štěpnička, Petr'
_publ_section_title
;
 Synthesis and structural characterisation of Group 11 metal complexes
 with a phosphinoferrocene oxazoline
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11450
_journal_paper_doi               10.1039/C8NJ02101E
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C54 H52 Cu2 Fe2 I2 N2 O2 P2'
_chemical_formula_sum            'C54 H52 Cu2 Fe2 I2 N2 O2 P2'
_chemical_formula_weight         1315.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                93.4567(10)
_cell_angle_beta                 104.9289(10)
_cell_angle_gamma                111.6134(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8304(3)
_cell_length_b                   10.1402(3)
_cell_length_c                   14.1354(3)
_cell_measurement_reflns_used    8133
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.44
_cell_volume                     1246.73(6)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2014.11.0.1'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.193
_exptl_absorpt_coefficient_mu    2.757
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       prism
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0248
_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/[σ²(Fo²)+(0.0222P)²+0.3733P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4980
_reflns_number_total             5719
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj02101e2.cif
_cod_data_source_block           md7
_cod_depositor_comments
'Adding full bibliography for 7057478--7057484.cif.'
_cod_database_code               7057479
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.421
_shelx_estimated_absorpt_t_max   0.699
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu Cu 0.65423(3) 0.00795(3) 0.57686(2) 0.01628(7) Uani 1 1 d . .
I I 0.63301(2) 0.16621(2) 0.43520(2) 0.01955(5) Uani 1 1 d . .
Fe Fe 0.82871(4) -0.18198(3) 0.82350(2) 0.01577(8) Uani 1 1 d . .
P P 0.80793(7) 0.12551(6) 0.72819(4) 0.01278(12) Uani 1 1 d . .
C1 C 0.9049(3) 0.0118(2) 0.77757(16) 0.0145(5) Uani 1 1 d . .
C2 C 0.9236(3) -0.0984(2) 0.71814(16) 0.0171(5) Uani 1 1 d . .
C3 C 1.0228(3) -0.1505(3) 0.78309(17) 0.0204(5) Uani 1 1 d . .
H3 H 1.055544 -0.222296 0.763862 0.025 Uiso 1 1 calc R U
C4 C 1.0637(3) -0.0763(2) 0.88122(17) 0.0189(5) Uani 1 1 d . .
H4 H 1.128147 -0.090158 0.939058 0.023 Uiso 1 1 calc R U
C5 C 0.9917(3) 0.0222(2) 0.87788(16) 0.0148(5) Uani 1 1 d . .
H5 H 0.999805 0.085111 0.933552 0.018 Uiso 1 1 calc R U
C6 C 0.6023(3) -0.2386(3) 0.8114(2) 0.0268(6) Uani 1 1 d . .
H6 H 0.545117 -0.181876 0.791379 0.032 Uiso 1 1 calc R U
C7 C 0.6191(3) -0.3399(3) 0.74832(19) 0.0307(6) Uani 1 1 d . .
H7 H 0.574633 -0.363959 0.678184 0.037 Uiso 1 1 calc R U
C8 C 0.7134(3) -0.4000(3) 0.8068(2) 0.0337(7) Uani 1 1 d . .
H8 H 0.744415 -0.470613 0.783121 0.040 Uiso 1 1 calc R U
C9 C 0.7534(3) -0.3356(3) 0.9076(2) 0.0327(7) Uani 1 1 d . .
H9 H 0.815139 -0.356390 0.963386 0.039 Uiso 1 1 calc R U
C10 C 0.6856(3) -0.2356(3) 0.91011(19) 0.0304(6) Uani 1 1 d . .
H10 H 0.694095 -0.176465 0.967898 0.037 Uiso 1 1 calc R U
O11 O 0.8954(2) -0.2609(2) 0.58129(12) 0.0335(5) Uani 1 1 d . .
C12 C 0.8509(3) -0.1589(2) 0.61207(17) 0.0189(5) Uani 1 1 d . .
N13 N 0.7562(2) -0.1272(2) 0.54746(13) 0.0173(4) Uani 1 1 d . .
C14 C 0.7285(3) -0.2129(3) 0.44881(17) 0.0222(5) Uani 1 1 d . .
C15 C 0.7970(4) -0.3214(3) 0.47914(19) 0.0409(8) Uani 1 1 d . .
H15A H 0.715489 -0.416490 0.475814 0.049 Uiso 1 1 calc R U
H15B H 0.857606 -0.332586 0.435452 0.049 Uiso 1 1 calc R U
C16 C 0.8144(4) -0.1113(3) 0.38970(19) 0.0352(7) Uani 1 1 d . .
H16A H 0.786379 -0.028044 0.387584 0.053 Uiso 1 1 calc R U
H16B H 0.787254 -0.161698 0.321851 0.053 Uiso 1 1 calc R U
H16C H 0.925125 -0.078626 0.421438 0.053 Uiso 1 1 calc R U
C17 C 0.5582(3) -0.2846(3) 0.3928(2) 0.0340(7) Uani 1 1 d . .
H17A H 0.503825 -0.344882 0.433913 0.051 Uiso 1 1 calc R U
H17B H 0.542944 -0.344570 0.330793 0.051 Uiso 1 1 calc R U
H17C H 0.518033 -0.210561 0.377411 0.051 Uiso 1 1 calc R U
C21 C 0.9704(3) 0.2929(2) 0.73411(15) 0.0140(5) Uani 1 1 d . .
C22 C 1.1219(3) 0.3265(2) 0.79074(17) 0.0179(5) Uani 1 1 d . .
H22 H 1.145568 0.259969 0.829467 0.021 Uiso 1 1 calc R U
C23 C 1.2379(3) 0.4559(3) 0.79084(18) 0.0212(5) Uani 1 1 d . .
H23 H 1.340339 0.478167 0.830189 0.025 Uiso 1 1 calc R U
C24 C 1.2050(3) 0.5530(3) 0.73368(18) 0.0223(5) Uani 1 1 d . .
H24 H 1.284839 0.641370 0.733441 0.027 Uiso 1 1 calc R U
C25 C 1.0564(3) 0.5208(2) 0.67728(17) 0.0214(5) Uani 1 1 d . .
H25 H 1.033882 0.587432 0.638162 0.026 Uiso 1 1 calc R U
C26 C 0.9389(3) 0.3918(2) 0.67714(16) 0.0178(5) Uani 1 1 d . .
H26 H 0.836721 0.370738 0.638041 0.021 Uiso 1 1 calc R U
C27 C 0.7431(3) 0.1770(2) 0.83011(16) 0.0158(5) Uani 1 1 d . .
C28 C 0.5886(3) 0.1105(3) 0.82341(19) 0.0268(6) Uani 1 1 d . .
H28 H 0.519330 0.040280 0.766901 0.032 Uiso 1 1 calc R U
C29 C 0.5350(3) 0.1460(3) 0.8987(2) 0.0392(8) Uani 1 1 d . .
H29 H 0.429254 0.099559 0.893399 0.047 Uiso 1 1 calc R U
C30 C 0.6339(3) 0.2485(3) 0.9814(2) 0.0342(7) Uani 1 1 d . .
H30 H 0.596800 0.271200 1.033292 0.041 Uiso 1 1 calc R U
C31 C 0.7865(3) 0.3173(3) 0.98780(18) 0.0255(6) Uani 1 1 d . .
H31 H 0.854737 0.388885 1.043850 0.031 Uiso 1 1 calc R U
C32 C 0.8408(3) 0.2825(2) 0.91263(17) 0.0192(5) Uani 1 1 d . .
H32 H 0.946071 0.331263 0.917477 0.023 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
N13 Cu P 100.94(6) .
N13 Cu I 110.45(5) .
P Cu I 116.636(19) .
N13 Cu I 105.09(6) 2_656
P Cu I 116.352(18) 2_656
I Cu I 106.625(11) 2_656
Cu I Cu 73.376(11) 2_656
C2 Fe C6 123.39(10) .
C2 Fe C1 41.85(8) .
C6 Fe C1 107.56(10) .
C2 Fe C5 69.18(9) .
C6 Fe C5 123.33(10) .
C1 Fe C5 40.96(9) .
C2 Fe C7 105.83(10) .
C6 Fe C7 40.17(11) .
C1 Fe C7 120.93(10) .
C5 Fe C7 157.73(11) .
C2 Fe C10 161.28(11) .
C6 Fe C10 40.58(10) .
C1 Fe C10 124.91(10) .
C5 Fe C10 109.58(10) .
C7 Fe C10 67.85(11) .
C2 Fe C8 119.40(10) .
C6 Fe C8 67.99(11) .
C1 Fe C8 156.03(10) .
C5 Fe C8 161.06(11) .
C7 Fe C8 40.46(11) .
C10 Fe C8 68.04(11) .
C2 Fe C3 41.13(9) .
C6 Fe C3 159.83(10) .
C1 Fe C3 69.44(9) .
C5 Fe C3 68.28(9) .
C7 Fe C3 123.04(11) .
C10 Fe C3 157.13(11) .
C8 Fe C3 106.21(11) .
C2 Fe C9 155.67(11) .
C6 Fe C9 67.87(11) .
C1 Fe C9 161.68(10) .
C5 Fe C9 125.47(10) .
C7 Fe C9 67.87(11) .
C10 Fe C9 40.19(12) .
C8 Fe C9 40.58(11) .
C3 Fe C9 121.14(11) .
C2 Fe C4 68.86(9) .
C6 Fe C4 158.74(10) .
C1 Fe C4 68.90(9) .
C5 Fe C4 40.39(9) .
C7 Fe C4 159.85(11) .
C10 Fe C4 123.10(10) .
C8 Fe C4 123.87(11) .
C3 Fe C4 40.40(9) .
C9 Fe C4 108.52(10) .
C1 P C21 101.58(10) .
C1 P C27 104.22(10) .
C21 P C27 101.10(10) .
C1 P Cu 105.53(7) .
C21 P Cu 116.62(7) .
C27 P Cu 124.93(8) .
C5 C1 C2 106.52(19) .
C5 C1 P 128.11(16) .
C2 C1 P 125.01(16) .
C5 C1 Fe 69.60(13) .
C2 C1 Fe 68.42(13) .
P C1 Fe 132.05(12) .
C3 C2 C1 107.86(19) .
C3 C2 C12 122.8(2) .
C1 C2 C12 129.2(2) .
C3 C2 Fe 70.44(13) .
C1 C2 Fe 69.73(12) .
C12 C2 Fe 122.38(17) .
C4 C3 C2 108.2(2) .
C4 C3 Fe 70.25(14) .
C2 C3 Fe 68.43(13) .
C4 C3 H3 125.9 .
C2 C3 H3 125.9 .
Fe C3 H3 127.0 .
C5 C4 C3 108.1(2) .
C5 C4 Fe 69.09(13) .
C3 C4 Fe 69.35(14) .
C5 C4 H4 125.9 .
C3 C4 H4 125.9 .
Fe C4 H4 127.2 .
C4 C5 C1 109.26(19) .
C4 C5 Fe 70.51(13) .
C1 C5 Fe 69.43(12) .
C4 C5 H5 125.4 .
C1 C5 H5 125.4 .
Fe C5 H5 126.3 .
C7 C6 C10 108.0(2) .
C7 C6 Fe 70.03(15) .
C10 C6 Fe 69.86(15) .
C7 C6 H6 126.0 .
C10 C6 H6 126.0 .
Fe C6 H6 125.7 .
C6 C7 C8 108.4(2) .
C6 C7 Fe 69.80(14) .
C8 C7 Fe 69.83(15) .
C6 C7 H7 125.8 .
C8 C7 H7 125.8 .
Fe C7 H7 126.2 .
C7 C8 C9 107.6(3) .
C7 C8 Fe 69.71(15) .
C9 C8 Fe 70.01(15) .
C7 C8 H8 126.2 .
C9 C8 H8 126.2 .
Fe C8 H8 125.6 .
C10 C9 C8 108.0(2) .
C10 C9 Fe 69.58(15) .
C8 C9 Fe 69.41(15) .
C10 C9 H9 126.0 .
C8 C9 H9 126.0 .
Fe C9 H9 126.6 .
C9 C10 C6 108.0(2) .
C9 C10 Fe 70.23(15) .
C6 C10 Fe 69.56(14) .
C9 C10 H10 126.0 .
C6 C10 H10 126.0 .
Fe C10 H10 125.8 .
C12 O11 C15 105.20(19) .
N13 C12 O11 117.64(19) .
N13 C12 C2 129.2(2) .
O11 C12 C2 113.1(2) .
C12 N13 C14 107.12(18) .
C12 N13 Cu 125.38(14) .
C14 N13 Cu 127.43(15) .
N13 C14 C16 107.94(19) .
N13 C14 C15 102.20(19) .
C16 C14 C15 112.1(2) .
N13 C14 C17 111.17(19) .
C16 C14 C17 110.7(2) .
C15 C14 C17 112.3(2) .
O11 C15 C14 104.59(19) .
O11 C15 H15A 110.8 .
C14 C15 H15A 110.8 .
O11 C15 H15B 110.8 .
C14 C15 H15B 110.8 .
H15A C15 H15B 108.9 .
C14 C16 H16A 109.5 .
C14 C16 H16B 109.5 .
H16A C16 H16B 109.5 .
C14 C16 H16C 109.5 .
H16A C16 H16C 109.5 .
H16B C16 H16C 109.5 .
C14 C17 H17A 109.5 .
C14 C17 H17B 109.5 .
H17A C17 H17B 109.5 .
C14 C17 H17C 109.5 .
H17A C17 H17C 109.5 .
H17B C17 H17C 109.5 .
C26 C21 C22 118.6(2) .
C26 C21 P 116.99(17) .
C22 C21 P 124.41(18) .
C23 C22 C21 120.6(2) .
C23 C22 H22 119.7 .
C21 C22 H22 119.7 .
C22 C23 C24 120.2(2) .
C22 C23 H23 119.9 .
C24 C23 H23 119.9 .
C25 C24 C23 119.8(2) .
C25 C24 H24 120.1 .
C23 C24 H24 120.1 .
C24 C25 C26 120.5(2) .
C24 C25 H25 119.7 .
C26 C25 H25 119.7 .
C25 C26 C21 120.4(2) .
C25 C26 H26 119.8 .
C21 C26 H26 119.8 .
C28 C27 C32 118.3(2) .
C28 C27 P 118.57(17) .
C32 C27 P 123.08(18) .
C29 C28 C27 120.4(2) .
C29 C28 H28 119.8 .
C27 C28 H28 119.8 .
C30 C29 C28 120.7(3) .
C30 C29 H29 119.7 .
C28 C29 H29 119.7 .
C31 C30 C29 119.4(2) .
C31 C30 H30 120.3 .
C29 C30 H30 120.3 .
C30 C31 C32 120.2(2) .
C30 C31 H31 119.9 .
C32 C31 H31 119.9 .
C31 C32 C27 120.9(2) .
C31 C32 H32 119.5 .
C27 C32 H32 119.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N13 2.0528(19) .
Cu P 2.2316(6) .
Cu I 2.6548(3) .
Cu I 2.6764(3) 2_656
Fe C2 2.023(2) .
Fe C6 2.040(3) .
Fe C1 2.041(2) .
Fe C5 2.043(2) .
Fe C7 2.043(3) .
Fe C10 2.044(3) .
Fe C8 2.045(3) .
Fe C3 2.050(2) .
Fe C9 2.053(3) .
Fe C4 2.062(2) .
P C1 1.814(2) .
P C21 1.832(2) .
P C27 1.839(2) .
C1 C5 1.429(3) .
C1 C2 1.452(3) .
C2 C3 1.431(3) .
C2 C12 1.466(3) .
C3 C4 1.420(3) .
C3 H3 0.9500 .
C4 C5 1.417(3) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C7 1.402(4) .
C6 C10 1.416(4) .
C6 H6 0.9500 .
C7 C8 1.413(4) .
C7 H7 0.9500 .
C8 C9 1.421(4) .
C8 H8 0.9500 .
C9 C10 1.408(4) .
C9 H9 0.9500 .
C10 H10 0.9500 .
O11 C12 1.352(3) .
O11 C15 1.461(3) .
C12 N13 1.273(3) .
N13 C14 1.502(3) .
C14 C16 1.516(4) .
C14 C15 1.517(4) .
C14 C17 1.520(4) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C21 C26 1.395(3) .
C21 C22 1.399(3) .
C22 C23 1.385(3) .
C22 H22 0.9500 .
C23 C24 1.387(3) .
C23 H23 0.9500 .
C24 C25 1.377(3) .
C24 H24 0.9500 .
C25 C26 1.390(3) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C27 C28 1.391(3) .
C27 C32 1.394(3) .
C28 C29 1.386(3) .
C28 H28 0.9500 .
C29 C30 1.384(4) .
C29 H29 0.9500 .
C30 C31 1.377(4) .
C30 H30 0.9500 .
C31 C32 1.387(3) .
C31 H31 0.9500 .
C32 H32 0.9500 .
