#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/48/2004827.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2004827
loop_
_publ_author_name
'Alcock, N. W.'
'Busch, D. H.'
'Vance, A. L.'
_publ_section_title
;
 A Copper(II) Complex of a Macrocyclic Schiff Base Ligand with a
 Polyether Bridge
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1134
_journal_page_last               1136
_journal_paper_doi               10.1107/S0108270196001278
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac
'[Cu Cl (H2 O) (C17 H25 N3 O3)] P F6 , C H3 C N'
_chemical_formula_sum            'C17 H27 Cl Cu F6 N3 O4 P'
_chemical_formula_weight         581.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           55
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a m'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.618(9)
_cell_length_b                   8.950(4)
_cell_length_c                   10.889(4)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      13
_cell_volume                     2594.1(17)
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m four circle diffractometer'
_diffrn_measurement_method       ω--2θ
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3139
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   'analytical (ABSPSI; Alcock & Marks, 1994)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plates
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.543
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2429
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.034
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_obs          0.0584
_refine_ls_shift/esd_max         -0.471
_refine_ls_shift/esd_mean        0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1002P)²+5.0808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1768
_refine_ls_wR_factor_obs         0.1554
_reflns_number_observed          1847
_reflns_number_total             2431
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1348.cif
_cod_data_source_block           vancubab
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

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

'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (4
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (7 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not neasured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.1002P)^2^+5.0808P] 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^)+(0.1002P)^2^+5.0808P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2004827
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_occupancy
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 1 .07268(3) .00673(8) .0000 .0386(3) Uani d S . Cu
Cl1 1 .02604(7) -0.1984(2) .0000 .0567(5) Uani d S . Cl
O1 1 .1456(2) -0.1190(5) .0000 .0409(10) Uani d SD . O
H01 1 .1642(16) -.099(6) .062(4) .056(16) Uiso d D . H
N1 1 .0952(2) .2137(5) .0000 .0357(11) Uani d S . N
C2 1 .1007(2) .2835(5) .1060(4) .0420(10) Uani d . . C
C3 1 .1137(2) .4341(5) .1093(5) .0556(13) Uani d . . C
H3 1 .1182(2) .4835(5) .1836(5) .080 Uiso calc R . H
C4 1 .1196(3) .5073(8) .0000 .062(2) Uani d S . C
H4 1 .1278(3) .6083(8) .0000 .080 Uiso calc SR . H
C5 1 .0914(2) .1850(5) .2116(5) .0491(12) Uani d . . C
H5 1 .0948(2) .2189(5) .2919(5) .080 Uiso calc R . H
N6 1 .07859(14) .0527(4) .1883(4) .0430(9) Uani d . . N
C7 1 .0727(2) -.0529(7) .2905(5) .0603(14) Uani d . . C
H7A 1 .0424(2) -0.1113(7) .2785(5) .080 Uiso calc R . H
H7B 1 .0693(2) .0020(7) .3669(5) .080 Uiso calc R . H
C8 1 .1180(2) -0.1573(6) .2989(5) .0628(15) Uani d . . C
H8A 1 .1118(2) -0.2283(6) .3645(5) .080 Uiso calc R . H
H8B 1 .1200(2) -0.2137(6) .2230(5) .080 Uiso calc R . H
C9 1 .1683(2) -.0854(7) .3213(5) .068(2) Uani d . . C
H9A 1 .1655(2) -.0126(7) .3869(5) .080 Uiso calc R . H
H9B 1 .1924(2) -0.1607(7) .3462(5) .080 Uiso calc R . H
O10 1 .18504(14) -.0141(4) .2122(3) .0574(9) Uani d . . O
C11 1 .2348(2) .0462(7) .2179(6) .069(2) Uani d . . C
H11A 1 .2592(2) -.0341(7) .2200(6) .080 Uiso calc R . H
H11B 1 .2387(2) .1056(7) .2918(6) .080 Uiso calc R . H
C12 1 .2428(2) .1394(6) .1093(6) .070(2) Uani d . . C
H12A 1 .2170(2) .2156(6) .1055(6) .080 Uiso calc R . H
H12B 1 .2751(2) .1890(6) .1159(6) .080 Uiso calc R . H
O13 1 .2416(2) .0529(6) .0000 .0602(14) Uani d S . O
P1 1 .16448(8) .4116(2) .5000 .0558(5) Uani d SD . P
F1 1 .1297(3) .2672(8) .5000 .122(3) Uani d SD . F
F21 .781(10) .1928(5) .5595(10) .5000 .146(5) Uani d SPD 1 F
F31 .781(10) .1835(3) .3341(10) .3791(9) .165(5) Uani d PD 1 F
F41 .781(10) .1275(6) .4899(9) .4124(12) .220(6) Uani d PD 1 F
F22 .219(10) .2221(9) .460(4) .5000 .080(8) Uiso d SPD 2 F
F32 .219(10) .2161(5) .3410(17) .4677(15) .073(6) Uiso d PD 2 F
F42 .219(10) .1586(7) .450(2) .3704(15) .065(5) Uiso d PD 2 F
O002 .50 .0000 .245(2) .5000 .098(4) Uiso d SP . O
O003 .50 .0000(6) -0.331(2) .4163(15) .164(6) Uiso d P . O
O004 .25 .0047(9) -0.454(2) .3073(18) .093(6) Uiso d P . O
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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Cu1 N6 . . 77.89(11) y
N1 Cu1 N6 . 6 77.89(11) ?
N6 Cu1 N6 . 6 155.8(2) y
N1 Cu1 Cl1 . . 163.9(2) y
N6 Cu1 Cl1 . . 101.80(11) y
N6 Cu1 Cl1 6 . 101.80(11) ?
N1 Cu1 O1 . . 102.1(2) y
N6 Cu1 O1 . . 91.91(11) y
N6 Cu1 O1 6 . 91.91(11) ?
Cl1 Cu1 O1 . . 93.96(13) y
C2 N1 C2 6 . 121.8(5) ?
C2 N1 Cu1 6 . 119.0(3) ?
C2 N1 Cu1 . . 119.0(3) ?
N1 C2 C3 . . 120.5(5) ?
N1 C2 C5 . . 112.4(4) ?
C3 C2 C5 . . 127.0(5) ?
C4 C3 C2 . . 118.0(5) ?
C3 C4 C3 6 . 120.9(7) ?
N6 C5 C2 . . 116.9(4) ?
C5 N6 C7 . . 118.8(5) ?
C5 N6 Cu1 . . 113.7(3) ?
C7 N6 Cu1 . . 127.4(4) ?
N6 C7 C8 . . 110.8(4) ?
C9 C8 C7 . . 116.7(5) ?
O10 C9 C8 . . 109.6(4) ?
C9 O10 C11 . . 115.0(4) ?
O10 C11 C12 . . 108.4(5) ?
O13 C12 C11 . . 111.3(5) ?
C12 O13 C12 . 6 113.9(6) ?
F42 P1 F42 6_556 . 149.9(17) ?
F42 P1 F32 6_556 6_556 88.4(9) ?
F42 P1 F32 . 6_556 114.2(11) ?
F42 P1 F32 6_556 . 114.2(11) ?
F42 P1 F32 . . 88.4(9) ?
F32 P1 F32 6_556 . 26.2(12) ?
F21 P1 F41 . . 85.5(6) ?
F21 P1 F41 . 6_556 85.5(6) ?
F41 P1 F41 . 6_556 76.6(12) ?
F21 P1 F31 . . 103.0(4) ?
F41 P1 F31 . . 83.5(6) ?
F41 P1 F31 6_556 . 157.7(9) ?
F21 P1 F31 . 6_556 103.0(4) ?
F41 P1 F31 . 6_556 157.7(9) ?
F41 P1 F31 6_556 6_556 83.5(6) ?
F31 P1 F31 . 6_556 113.8(9) ?
F42 P1 F1 6_556 . 97.4(7) ?
F42 P1 F1 . . 97.4(7) ?
F21 P1 F1 . . 174.1(6) ?
F32 P1 F1 6_556 . 100.6(7) ?
F32 P1 F1 . . 100.6(7) ?
F41 P1 F1 . . 89.8(6) ?
F41 P1 F1 6_556 . 89.8(6) ?
F31 P1 F1 . . 80.1(3) ?
F31 P1 F1 6_556 . 80.1(3) ?
F42 P1 F22 6_556 . 92.2(7) ?
F42 P1 F22 . . 92.2(7) ?
F32 P1 F22 6_556 . 42.2(12) ?
F32 P1 F22 . . 42.2(12) ?
F1 P1 F22 . . 141.4(13) ?
F32 F22 F32 . 6_556 36.1(19) ?
F32 F22 P1 . . 66.9(14) ?
F32 F22 P1 6_556 . 66.9(14) ?
F32 F32 F22 6_556 . 71.9(9) ?
F32 F32 P1 6_556 . 76.9(6) ?
F22 F32 P1 . . 70.9(14) ?
O003 O002 O003 2 5_556 100.(2) ?
O002 O003 O004 5_556 . 174.7(17) ?
O002 O003 O003 5_556 6_556 40.0(11) ?
O004 O003 O003 . 6_556 136.9(10) ?
O004 O004 O003 2_545 . 128.9(15) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N1 . 1.947(5) y
Cu1 N6 . 2.098(4) y
Cu1 N6 6 2.098(4) ?
Cu1 Cl1 . 2.217(2) y
Cu1 O1 . 2.244(5) y
N1 C2 6 1.320(5) ?
N1 C2 . 1.320(5) ?
C2 C3 . 1.392(7) ?
C2 C5 . 1.471(7) ?
C3 C4 . 1.367(6) ?
C4 C3 6 1.367(6) ?
C5 N6 . 1.258(6) ?
N6 C7 . 1.468(7) ?
C7 C8 . 1.527(8) ?
C8 C9 . 1.506(8) ?
C9 O10 . 1.421(7) ?
O10 C11 . 1.431(7) ?
C11 C12 . 1.463(9) ?
C12 O13 . 1.420(6) ?
O13 C12 6 1.420(6) ?
P1 F42 6_556 1.46(2) ?
P1 F42 . 1.46(2) ?
P1 F21 . 1.524(7) ?
P1 F32 6_556 1.552(14) ?
P1 F32 . 1.552(13) ?
P1 F41 . 1.540(8) ?
P1 F41 6_556 1.540(8) ?
P1 F31 . 1.572(7) ?
P1 F31 6_556 1.572(7) ?
P1 F1 . 1.590(6) ?
P1 F22 . 1.59(2) ?
F22 F32 . 1.13(3) ?
F22 F32 6_556 1.13(3) ?
F32 F32 6_556 0.70(3) ?
O002 O003 2 1.19(2) ?
O002 O003 5_556 1.19(2) ?
O003 O002 5_556 1.19(2) ?
O003 O004 . 1.63(3) ?
O003 O003 6_556 1.82(3) ?
O004 O004 2_545 0.86(4) ?
