#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/88/7018872.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_7018872
loop_
_publ_author_name
'Gould, Jamie A.'
'Rosseinsky, Matthew J.'
'Moggach, Stephen A.'
_publ_section_title
;
 Tuning the coordination chemistry of a Cu(ii) complex at high-pressure.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5464
_journal_page_last               5467
_journal_paper_doi               10.1039/c2dt12302a
_journal_volume                  41
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C4 H9 Cu1 N1 O6'
_chemical_formula_sum            'C4 H9 Cu N O6'
_chemical_formula_weight         230.66
_chemical_name_common            CuAsp
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             11-07-11
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 93.856(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4817(3)
_cell_length_b                   10.0118(3)
_cell_length_c                   7.5433(7)
_cell_measurement_reflns_used    1800
_cell_measurement_temperature    293
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     714.46(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_pressure         300000
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.423
_diffrn_measured_fraction_theta_max 0.406
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ' synchrotron'
_diffrn_radiation_wavelength     0.47620
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            2706
_diffrn_reflns_theta_full        25.564
_diffrn_reflns_theta_max         30.433
_diffrn_reflns_theta_min         2.962
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.049
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.94
_refine_ls_abs_structure_details 'Flack (1983), 390 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.27(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         846
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.0001454
_refine_ls_shift/su_mean         0.0000206
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
6.83 8.61 2.63
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0873
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0873
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              4
_reflns_limit_l_min              0
_reflns_number_gt                639
_reflns_number_total             855
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0397
_oxford_refine_ls_scale          0.3115(6)
_oxford_reflns_number_all        846
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ceth01 in C2'
_cod_data_source_file            c2dt12302a.txt
_cod_data_source_block           ceth01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C4 H9 Cu1 N1 O6'
_cod_database_code               7018872
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S
CONT CU(1, U'S)
CONT C(1, U[ISO]) UNTIL N(1)
CONT ENANTIO
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE O ( 5,X'S) H ( 51,X'S) H ( 52,X'S)
RIDE O ( 6,X'S) H ( 61,X'S) H ( 62,X'S)
RIDE N ( 1,X'S) H ( 11,X'S) H ( 12,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
DIST 0.84, 0.01 = O(6) TO H(61)
DIST 0.84, 0.01 = O(6) TO H(62)
ANGLE 108, 1 = H(61) TO O(6) TO H(62)
DIST 0.84, 0.01 = O(5) TO H(51)
DIST 0.84, 0.01 = O(5) TO H(52)

ANGLE 108, 1 = H(51) TO O(5) TO H(52)
DIST 1.292, 0.01 = C(1) TO O(1)
DIST 1.232, 0.01 = C(1) TO O(2)
DIST 1.525, 0.01 = C(1) TO C(2)
DIST 1.489, 0.01 = C(2) TO N(1)
DIST 1.514, 0.01 = C(2) TO C(3)
DIST 1.528, 0.01 = C(3) TO C(4)
DIST 1.280, 0.01 = C(4) TO O(3)
DIST 1.239, 0.01 = C(4) TO O(4)
ANGL 123,1= O(2) TO C(1) TO O(1)
ANGL 118,1= C(2) TO C(1) TO O(1)
ANGL 120,1= C(2) TO C(1) TO O(2)
ANGL 109,1= C(1) TO C(2) TO N(1)
ANGL 110,1= C(3) TO C(2) TO N(1)
ANGL 110,1= C(3) TO C(2) TO C(1)
ANGL 115,1= C(4) TO C(3) TO C(2)
ANGL 124,1= O(4) TO C(4) TO O(3)
ANGL 114,1= C(3) TO C(4) TO O(3)
ANGL 122,1= C(3) TO C(4) TO O(4)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = O(1) TO C(1)
VIBR .0, 0.00200 = O(2) TO C(1)
VIBR .0, 0.00200 = O(3) TO C(4)
VIBR .0, 0.00200 = O(4) TO C(4)
VIBR .0, 0.00200 = N(1) TO C(2)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00500 = O(2) TO O(1)
VIBR .0, 0.00500 = C(2) TO O(1)
VIBR .0, 0.00500 = C(2) TO O(2)
VIBR .0, 0.00200 = C(2) TO C(3)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = C(3) TO C(1)
VIBR .0, 0.00500 = C(3) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00500 = C(4) TO C(2)
VIBR .0, 0.00500 = O(3) TO C(3)
VIBR .0, 0.00500 = O(4) TO C(3)
VIBR .0, 0.00500 = O(4) TO O(3)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = O(1) TO C(1)
U(IJ) .0, 0.08000 = O(2) TO C(1)
U(IJ) .0, 0.08000 = O(3) TO C(4)
U(IJ) .0, 0.08000 = O(4) TO C(4)
U(IJ) .0, 0.08000 = N(1) TO C(2)
U(IJ) .0, 0.04000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO C(3)
U(IJ) .0, 0.04000 = C(3) TO C(4)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
DISTANCE 0.840000 , 0.010000 = O(5) TO H(52)
END
;
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.23687(5) 1.00279(15) 0.87375(19) 0.0221 1.0000 Uani . .
C1 C 0.3215(5) 0.7814(4) 0.6847(10) 0.0181(8) 1.0000 Uiso D U
C2 C 0.2257(4) 0.8541(4) 0.5467(10) 0.0161(8) 1.0000 Uiso D U
C3 C 0.3137(5) 0.9156(5) 0.4096(11) 0.0163(8) 1.0000 Uiso D U
C4 C 0.2383(4) 0.9416(5) 0.2298(10) 0.0166(8) 1.0000 Uiso D U
O1 O 0.3301(4) 0.8297(4) 0.8439(11) 0.0234(8) 1.0000 Uiso D U
O2 O 0.3900(4) 0.6836(4) 0.6421(12) 0.0199(8) 1.0000 Uiso D U
O3 O 0.3073(3) 1.0113(5) 0.1250(10) 0.0188(7) 1.0000 Uiso D U
O4 O 0.1186(4) 0.8943(4) 0.1920(12) 0.0188(8) 1.0000 Uiso D U
O5 O 0.1281(4) 1.1683(4) 0.8768(14) 0.0211(9) 1.0000 Uiso D .
O6 O 0.4276(4) 1.1177(4) 0.7749(14) 0.0220(9) 1.0000 Uiso D .
N1 N 0.1450(4) 0.9591(4) 0.6364(14) 0.0168(8) 1.0000 Uiso D U
H61 H 0.4278 1.1986 0.8044 0.0269 1.0000 Uiso DR .
H62 H 0.5044 1.0833 0.8149 0.0269 1.0000 Uiso DR .
H51 H 0.1217 1.1941 0.9821 0.0251 1.0000 Uiso DR .
H52 H 0.0470 1.1485 0.8342 0.0251 1.0000 Uiso DR .
H31 H 0.3495 1.0003 0.4560 0.0195 1.0000 Uiso R .
H32 H 0.3923 0.8560 0.3923 0.0195 1.0000 Uiso R .
H21 H 0.1594 0.7901 0.4886 0.0193 1.0000 Uiso R .
H11 H 0.1412 1.0299 0.5718 0.0201 1.0000 Uiso R .
H12 H 0.0607 0.9306 0.6491 0.0201 1.0000 Uiso R .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0163(2) 0.0141(3) 0.0351(19) -0.0005(5) -0.0040(3) 0.0025(2)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 1_556 Cu1 O1 . 91.3(3) yes
O3 1_556 Cu1 O5 . 95.6(3) yes
O1 . Cu1 O5 . 172.6(3) yes
O3 1_556 Cu1 O6 . 93.8(3) yes
O1 . Cu1 O6 . 91.97(18) yes
O5 . Cu1 O6 . 90.39(19) yes
O3 1_556 Cu1 N1 . 167.7(2) yes
O1 . Cu1 N1 . 82.9(3) yes
O5 . Cu1 N1 . 89.9(3) yes
O6 . Cu1 N1 . 97.1(3) yes
C2 . C1 O1 . 117.1(4) yes
C2 . C1 O2 . 120.3(5) yes
O1 . C1 O2 . 122.6(5) yes
C1 . C2 C3 . 109.5(4) yes
C1 . C2 N1 . 109.2(5) yes
C3 . C2 N1 . 110.4(4) yes
C1 . C2 H21 . 109.2 no
C3 . C2 H21 . 109.2 no
N1 . C2 H21 . 109.3 no
C2 . C3 C4 . 115.9(4) yes
C2 . C3 H31 . 107.9 no
C4 . C3 H31 . 107.9 no
C2 . C3 H32 . 107.9 no
C4 . C3 H32 . 107.9 no
H31 . C3 H32 . 109.5 no
C3 . C4 O3 . 114.9(4) yes
C3 . C4 O4 . 120.6(5) yes
O3 . C4 O4 . 124.5(6) yes
C1 . O1 Cu1 . 115.8(4) yes
C4 . O3 Cu1 1_554 114.8(3) yes
Cu1 . O5 H51 . 110.1 no
Cu1 . O5 H52 . 105.5 no
H51 . O5 H52 . 108.2 no
Cu1 . O6 H61 . 112.5 no
Cu1 . O6 H62 . 110.9 no
H61 . O6 H62 . 108.2 no
C2 . N1 Cu1 . 110.9(4) yes
C2 . N1 H11 . 109.1 no
Cu1 . N1 H11 . 109.1 no
C2 . N1 H12 . 109.1 no
Cu1 . N1 H12 . 109.1 no
H11 . N1 H12 . 109.5 no
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 O3 1_556 1.968(7) yes
Cu1 O1 . 1.965(4) yes
Cu1 O5 . 1.953(4) yes
Cu1 O6 . 2.309(6) yes
Cu1 N1 . 1.987(10) yes
C1 C2 . 1.520(7) yes
C1 O1 . 1.292(8) yes
C1 O2 . 1.230(6) yes
C2 C3 . 1.504(7) yes
C2 N1 . 1.490(7) yes
C2 H21 . 0.980 no
C3 C4 . 1.513(8) yes
C3 H31 . 0.970 no
C3 H32 . 0.970 no
C4 O3 . 1.269(7) yes
C4 O4 . 1.245(5) yes
O5 H51 . 0.842 no
O5 H52 . 0.837 no
O6 H61 . 0.840 no
O6 H62 . 0.843 no
N1 H11 . 0.860 no
N1 H12 . 0.860 no
#BEGIN Loops that were not found in dictionaries:
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
2 2 0 x
-4 -2 1 x
2 6 3 x
-7 -1 3 x
-7 3 3 x
2 10 4 x
4 10 4 x
-3 3 2 x
2 -4 0 x
#END Loops that were not found in dictionaries
