#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:33:23 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195024 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/78/7227818.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_7227818
loop_
_publ_author_name
'Bovill, Sally M.'
'Dixey, Richard J. C.'
'Saines, Paul J.'
_publ_section_title
;
 Three coordination frameworks with copper formate based low dimensional
 motifs: synthesis, structure and magnetic properties
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1831
_journal_paper_doi               10.1039/C6CE01601D
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C H7 Cl Cu N2 O6'
_chemical_formula_sum            'C H7 Cl Cu N2 O6'
_chemical_formula_weight         242.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_update_record
;
2017-01-25 deposited with the CCDC.
2017-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4087(6)
_cell_length_b                   7.8568(7)
_cell_length_c                   12.3745(10)
_cell_measurement_reflns_used    941
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     720.30(10)
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ω
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.04874
_diffrn_orient_matrix_UB_12      0.03084
_diffrn_orient_matrix_UB_13      -0.12203
_diffrn_orient_matrix_UB_21      0.11506
_diffrn_orient_matrix_UB_22      -0.01939
_diffrn_orient_matrix_UB_23      -0.05086
_diffrn_orient_matrix_UB_31      -0.01851
_diffrn_orient_matrix_UB_32      -0.07770
_diffrn_orient_matrix_UB_33      -0.01225
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         3.071
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_T_max  1.148
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.764
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.481
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1145P)²+0.7763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.2140
_reflns_d_resolution_high        0.62
_reflns_d_resolution_low         1.43
_reflns_Friedel_coverage         0.000
_reflns_number_gt                584
_reflns_number_total             879
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;

    shelx.res created by SHELXL-2014/7

TITL shelx in Pnma #62
REM reset to Pnma #62
CELL 0.71073 7.4087 7.8568 12.3745 90 90 90
ZERR 4 0.0006 0.0007 0.001 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC C H Cl Cu N O
UNIT 4 28 4 4 8 24
 
L.S. 10
PLAN  25
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./shelx.hkl">
REM </olex2.extras>
 
WGHT    0.114500    0.776300
FVAR       0.15918
CU1   4    0.168182    0.250000    0.356462    10.50000    0.01580    0.01486 =
         0.01262    0.00000    0.00128    0.00000
CL1   3    0.344241    0.250000    0.603154    10.50000    0.01559    0.01410 =
         0.01285    0.00000    0.00026    0.00000
O4    6    0.356015    0.250000    0.240245    10.50000    0.01729    0.01543 =
         0.01199    0.00000    0.00024    0.00000
N1    5    0.175086    0.503189    0.366989    11.00000    0.01344    0.01887 =
         0.02077    0.00558    0.00184    0.00040
AFIX 137
H1A   2    0.088612    0.547397    0.325702    11.00000   -1.20000
H1B   2    0.282089    0.540753    0.344633    11.00000   -1.20000
H1C   2    0.157637    0.534416    0.435331    11.00000   -1.20000
AFIX   0
C1    1    0.311641    0.250000    0.138342    10.50000    0.00969    0.01776 =
         0.01819    0.00000   -0.00544    0.00000
AFIX  43
H1    2    0.190035    0.250000    0.119701    10.50000   -1.20000
AFIX   0
O5    6    0.426352    0.250000    0.065547    10.50000    0.02015    0.01696 =
         0.01063    0.00000    0.00359    0.00000
 
O1    6    0.494134    0.250000    0.676183    10.50000    0.01362    0.03776 =
         0.01761    0.00000   -0.00723    0.00000
O2    6    0.239078    0.101033    0.619162    11.00000    0.02840    0.02258 =
         0.03212    0.00240   -0.00307   -0.01062
O3    6    0.413549    0.250000    0.494288    10.50000    0.01770    0.04252 =
         0.01223    0.00000   -0.00147    0.00000
HKLF 4
 
REM  shelx in Pnma #62
REM R1 =  0.0534 for     584 Fo > 4sig(Fo)  and  0.0969 for all     879 data
REM     62 parameters refined using      0 restraints
 
END  
     
WGHT      0.1144      0.7763 

REM Highest difference peak  1.764,  deepest hole -1.634,  1-sigma level  0.481
Q1    1   0.6644  0.2500  0.5632  10.50000  0.05    1.76
Q2    1   0.2648  0.7500  0.4488  10.50000  0.05    1.69
Q3    1   0.3191  0.2500 -0.0201  10.50000  0.05    1.57
Q4    1   0.2206  0.2500  0.0520  10.50000  0.05    1.49
Q5    1   0.2118  0.7500  0.3947  10.50000  0.05    1.25
Q6    1   0.3647  0.2500  0.1039  10.50000  0.05    1.16
Q7    1   0.5463  0.2500  0.6177  10.50000  0.05    1.14
Q8    1   0.2218  0.7500  0.3431  10.50000  0.05    1.12
Q9    1   0.0210  0.7500  0.3997  10.50000  0.05    1.10
Q10   1   0.5089  0.2500  0.7026  10.50000  0.05    1.06
Q11   1   0.4362  0.2500  0.0196  10.50000  0.05    1.01
Q12   1   0.0099  0.2500  0.1403  10.50000  0.05    1.00
Q13   1   0.2276  0.1249  0.0646  11.00000  0.05    1.00
Q14   1   0.1072  0.7500  0.3317  10.50000  0.05    0.90
Q15   1   0.4717  0.2500  0.0766  10.50000  0.05    0.85
Q16   1   0.2208  0.1017  0.6477  11.00000  0.05    0.84
Q17   1   0.1886  0.6427  0.3509  11.00000  0.05    0.78
Q18   1   0.3342  0.6181  0.3709  11.00000  0.05    0.74
Q19   1   0.3158  0.6949  0.3128  11.00000  0.05    0.70
Q20   1   0.6377  0.2500  0.7608  10.50000  0.05    0.64
Q21   1   0.4128  0.2500  0.2388  10.50000  0.05    0.62
Q22   1   0.4016 -0.0415  0.5299  11.00000  0.05    0.56
Q23   1   0.4717  0.1314  0.6611  11.00000  0.05    0.49
Q24   1   0.3526  0.2500  0.7093  10.50000  0.05    0.47
Q25   1   0.1381  0.1274  0.7309  11.00000  0.05    0.47

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0534 for 584 Fo > 4sig(Fo) and 0.0969 for all 988 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.76, deepest hole -1.63
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0969
  REM R1_gt = 0.0534
  REM wR_ref = 0.2140
  REM GOOF = 1.177
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 988
  REM Reflections_gt = 584
  REM Parameters = n/a
  REM Hole = -1.63
  REM Peak = 1.76
  REM Flack = n/a

  
;
_cod_data_source_file            c6ce01601d2.cif
_cod_data_source_block           CuFmClO4
_cod_depositor_comments
'Adding full bibliography for 7227816--7227818.cif.'
_cod_database_code               7227818
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
2.b Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.16818(18) 0.2500 0.35646(11) 0.0144(5) Uani 1 2 d S T P
Cl1 Cl 0.3442(3) 0.2500 0.6032(2) 0.0142(6) Uani 1 2 d S T P
O4 O 0.3560(11) 0.2500 0.2402(6) 0.0149(16) Uani 1 2 d S T P
N1 N 0.1751(8) 0.5032(9) 0.3670(5) 0.0177(14) Uani 1 1 d . . .
H1A H 0.0886 0.5474 0.3257 0.021 Uiso 1 1 calc GR . .
H1B H 0.2821 0.5408 0.3446 0.021 Uiso 1 1 calc GR . .
H1C H 0.1576 0.5344 0.4353 0.021 Uiso 1 1 calc GR . .
C1 C 0.3116(15) 0.2500 0.1383(9) 0.015(2) Uani 1 2 d S T P
H1 H 0.1900 0.2500 0.1197 0.018 Uiso 1 2 calc RS T P
O5 O 0.4264(10) 0.2500 0.0655(5) 0.0159(16) Uani 1 2 d S T P
O1 O 0.4941(11) 0.2500 0.6762(6) 0.0230(18) Uani 1 2 d S T P
O2 O 0.2391(9) 0.1010(8) 0.6192(5) 0.0277(14) Uani 1 1 d . . .
O3 O 0.4135(12) 0.2500 0.4943(6) 0.0242(19) Uani 1 2 d S T P
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 0.0158(8) 0.0149(7) 0.0126(7) 0.000 0.0013(5) 0.000
Cl1 0.0156(14) 0.0141(12) 0.0128(12) 0.000 0.0003(9) 0.000
O4 0.017(4) 0.015(4) 0.012(4) 0.000 0.000(3) 0.000
N1 0.013(3) 0.019(3) 0.021(3) 0.006(3) 0.002(3) 0.000(3)
C1 0.010(5) 0.018(5) 0.018(5) 0.000 -0.005(4) 0.000
O5 0.020(4) 0.017(4) 0.011(3) 0.000 0.004(3) 0.000
O1 0.014(4) 0.038(5) 0.018(4) 0.000 -0.007(3) 0.000
O2 0.028(3) 0.023(3) 0.032(3) 0.002(3) -0.003(3) -0.011(3)
O3 0.018(4) 0.043(5) 0.012(4) 0.000 -0.001(3) 0.000
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'
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'
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'
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
O4 Cu1 O5 162.4(3) . 6_556
N1 Cu1 O4 91.67(18) 8_565 .
N1 Cu1 O4 91.67(18) . .
N1 Cu1 N1 172.0(4) 8_565 .
N1 Cu1 O5 89.52(18) . 6_556
N1 Cu1 O5 89.52(18) 8_565 6_556
O1 Cl1 O3 108.3(5) . .
O2 Cl1 O1 109.7(3) 8_565 .
O2 Cl1 O1 109.7(3) . .
O2 Cl1 O2 111.0(6) . 8_565
O2 Cl1 O3 109.0(3) . .
O2 Cl1 O3 109.0(3) 8_565 .
C1 O4 Cu1 121.3(7) . .
Cu1 N1 H1A 109.5 . .
Cu1 N1 H1B 109.5 . .
Cu1 N1 H1C 109.5 . .
H1A N1 H1B 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
O4 C1 H1 119.0 . .
O5 C1 O4 122.1(10) . .
O5 C1 H1 119.0 . .
C1 O5 Cu1 105.0(6) . 6_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 2.001(7) .
Cu1 N1 1.994(7) 8_565
Cu1 N1 1.994(7) .
Cu1 O5 2.035(8) 6_556
Cl1 O1 1.432(8) .
Cl1 O2 1.420(6) .
Cl1 O2 1.420(6) 8_565
Cl1 O3 1.442(8) .
O4 C1 1.303(12) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
C1 H1 0.9300 .
C1 O5 1.238(13) .
O5 Cu1 2.035(8) 6_656
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
Cu1 O4 C1 O5 180.000(1) .
O4 C1 O5 Cu1 0.000(1) 6_656
