#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:36:45 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178659 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/70/4077021.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_4077021
loop_
_publ_author_name
'Kozlowski, Marisa C.'
'Li, Xiaolin'
'Carroll, Patrick J.'
'Xu, Zhenrong'
_publ_section_title
;
 Copper(II) Complexes of Novel 1,5-Diaza-cis-decalin Diamine
 Ligands:  An Investigation of Structure and Reactivity
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4513
_journal_paper_doi               10.1021/om020425p
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C22 H42 Cu2 F6 N4 O8 S2'
_chemical_formula_weight         795.80
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                99.93(2)
_cell_angle_beta                 92.063(6)
_cell_angle_gamma                79.584(14)
_cell_formula_units_Z            1
_cell_length_a                   8.798(2)
_cell_length_b                   12.136(2)
_cell_length_c                   7.922(2)
_cell_measurement_temperature    200(2)
_cell_volume                     819.4(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'image plate area detector'
_diffrn_measurement_device_type  'Rigaku R-AXIS IIc'
_diffrn_measurement_method       'phi oscillations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6412
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.0316(87)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.107
_refine_ls_goodness_of_fit_obs   1.141
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2717
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.139
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_obs          0.1168
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1625P)²+4.7513P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3172
_refine_ls_wR_factor_obs         0.3047
_reflns_number_observed          2364
_reflns_number_total             2717
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om020425p.cif
_cod_data_source_block           '[(2)Cu(OH)]2(OTf)2-UP821'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1625P)^2^+4.7513P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.1625P)^2^+4.7513P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        819.5(3)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_database_code               4077021
loop_
_symmetry_equiv_pos_as_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu Cu 0.90295(13) 0.59993(10) 0.4413(2) 0.0552(6) Uani 1 d . .
O1 O 1.0774(11) 0.5606(7) 0.5802(12) 0.089(3) Uani 1 d . .
H1 H 1.1384(11) 0.6082(7) 0.6434(12) 0.118 Uiso 1 calc R .
N1 N 0.9139(11) 0.7679(9) 0.4485(12) 0.073(3) Uani 1 d . .
N10 N 0.7057(12) 0.6321(9) 0.3112(15) 0.080(3) Uani 1 d . .
C2 C 0.8540(15) 0.8269(12) 0.6226(17) 0.081(4) Uani 1 d . .
H2A H 0.9315(15) 0.8086(12) 0.7083(17) 0.107 Uiso 1 calc R .
H2B H 0.8375(15) 0.9085(12) 0.6256(17) 0.107 Uiso 1 calc R .
C3 C 0.7135(16) 0.7960(13) 0.6649(16) 0.084(4) Uani 1 d . .
H3A H 0.6740(16) 0.8434(13) 0.7710(16) 0.111 Uiso 1 calc R .
H3B H 0.7339(16) 0.7176(13) 0.6832(16) 0.111 Uiso 1 calc R .
C4 C 0.5861(15) 0.8094(13) 0.5186(19) 0.087(4) Uani 1 d . .
H4A H 0.5046(15) 0.7682(13) 0.5351(19) 0.115 Uiso 1 calc R .
H4B H 0.5407(15) 0.8890(13) 0.5243(19) 0.115 Uiso 1 calc R .
C5 C 0.6582(13) 0.7645(12) 0.3504(16) 0.078(4) Uani 1 d . .
H5 H 0.5811(13) 0.7858(12) 0.2639(16) 0.103 Uiso 1 calc R .
C6 C 0.7981(14) 0.8062(11) 0.3142(16) 0.072(3) Uani 1 d . .
H6 H 0.7752(14) 0.8895(11) 0.3358(16) 0.096 Uiso 1 calc R .
C7 C 0.8546(18) 0.7685(12) 0.1364(17) 0.087(4) Uani 1 d . .
H7A H 0.9520(18) 0.7936(12) 0.1266(17) 0.116 Uiso 1 calc R .
H7B H 0.7811(18) 0.8047(12) 0.0596(17) 0.116 Uiso 1 calc R .
C8 C 0.8780(20) 0.6378(14) 0.0786(17) 0.098(5) Uani 1 d . .
H8A H 0.8877(20) 0.6197(14) -0.0451(17) 0.130 Uiso 1 calc R .
H8B H 0.9726(20) 0.6023(14) 0.1287(17) 0.130 Uiso 1 calc R .
C9 C 0.7451(18) 0.5925(14) 0.1330(21) 0.095(5) Uani 1 d . .
H9A H 0.6559(18) 0.6146(14) 0.0629(21) 0.126 Uiso 1 calc R .
H9B H 0.7697(18) 0.5101(14) 0.1131(21) 0.126 Uiso 1 calc R .
C11 C 1.0640(16) 0.7934(13) 0.4205(22) 0.094(4) Uani 1 d . .
H11A H 1.0566(31) 0.8741(15) 0.4299(147) 0.141 Uiso 1 calc R .
H11B H 1.0997(59) 0.7569(80) 0.3081(59) 0.141 Uiso 1 calc R .
H11C H 1.1355(36) 0.7663(88) 0.5049(91) 0.141 Uiso 1 calc R .
C12 C 0.5831(16) 0.5802(14) 0.3610(24) 0.105(5) Uani 1 d . .
H12A H 0.6179(52) 0.4997(18) 0.3512(156) 0.158 Uiso 1 calc R .
H12B H 0.4952(56) 0.5945(95) 0.2874(108) 0.158 Uiso 1 calc R .
H12C H 0.5546(101) 0.6117(77) 0.4775(59) 0.158 Uiso 1 calc R .
C13 C 0.2828(8) 0.9003(5) -0.0376(12) 0.095(5) Uani 1 d . .
F1 F 0.4005(8) 0.9359(5) 0.0495(19) 0.145(6) Uani 0.75 calc PRU 1
F2 F 0.1540(8) 0.9425(5) 0.0491(14) 0.092(3) Uani 0.75 calc PRU 1
F3 F 0.2722(16) 0.9347(5) -0.1875(12) 0.163(8) Uani 0.75 calc PRU 1
F1' F 0.3198(12) 0.9395(5) 0.1216(14) 0.163(12) Uani 0.25 calc PRU 2
F2' F 0.1363(9) 0.9407(5) -0.0661(14) 0.118(10) Uani 0.25 calc PRU 2
F3' F 0.3706(14) 0.9329(5) -0.1445(17) 0.154(12) Uani 0.25 calc PRU 2
S1 S 0.3127(3) 0.7464(2) -0.0703(3) 0.0661(8) Uani 1 d . .
O2 O 0.4585(5) 0.6998(2) -0.1598(9) 0.110(4) Uani 1 calc R .
O3 O 0.1858(6) 0.7069(2) -0.1728(9) 0.142(5) Uani 1 calc R .
O4 O 0.3180(9) 0.7086(2) 0.0954(4) 0.122(4) Uani 1 calc R .
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'
S S 0.1246 0.1234 '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'
F F 0.0171 0.0103 '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'
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_3
O1 Cu O1 77.0(4) . 2_766
O1 Cu N10 173.3(4) . .
O1 Cu N10 99.1(4) 2_766 .
O1 Cu N1 98.8(4) . .
O1 Cu N1 171.5(4) 2_766 .
N10 Cu N1 85.7(4) . .
O1 Cu Cu 38.6(3) . 2_766
O1 Cu Cu 38.4(2) 2_766 2_766
N10 Cu Cu 137.3(3) . 2_766
N1 Cu Cu 137.0(3) . 2_766
Cu O1 Cu 103.0(4) . 2_766
C11 N1 C2 110.3(11) . .
C11 N1 C6 111.2(10) . .
C2 N1 C6 108.4(9) . .
C11 N1 Cu 116.3(9) . .
C2 N1 Cu 105.3(8) . .
C6 N1 Cu 104.9(7) . .
C12 N10 C9 111.2(12) . .
C12 N10 C5 109.8(11) . .
C9 N10 C5 111.5(10) . .
C12 N10 Cu 114.3(8) . .
C9 N10 Cu 105.6(8) . .
C5 N10 Cu 104.2(7) . .
C3 C2 N1 113.0(11) . .
C2 C3 C4 112.1(11) . .
C5 C4 C3 109.4(10) . .
C6 C5 C4 117.0(13) . .
C6 C5 N10 104.2(10) . .
C4 C5 N10 114.6(11) . .
C5 C6 C7 114.4(12) . .
C5 C6 N1 104.3(10) . .
C7 C6 N1 113.7(10) . .
C6 C7 C8 113.4(11) . .
C9 C8 C7 110.3(13) . .
N10 C9 C8 113.2(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O1 1.894(8) .
Cu O1 1.903(8) 2_766
Cu N10 1.998(9) .
Cu N1 2.049(11) .
Cu Cu 2.972(2) 2_766
O1 Cu 1.903(8) 2_766
N1 C11 1.44(2) .
N1 C2 1.51(2) .
N1 C6 1.519(14) .
N10 C12 1.44(2) .
N10 C9 1.44(2) .
N10 C5 1.56(2) .
C2 C3 1.42(2) .
C3 C4 1.59(2) .
C4 C5 1.47(2) .
C5 C6 1.47(2) .
C6 C7 1.48(2) .
C7 C8 1.55(2) .
C8 C9 1.49(2) .
C13 S1 1.813(7) .
