#------------------------------------------------------------------------------
#$Date: 2017-04-05 11:33:23 +0200 (Wed 05 de Apr de 2017) $
#$Revision: 195024 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/78/7227817.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_7227817
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 Cu N3 O5'
_chemical_formula_sum            'C H7 Cu N3 O5'
_chemical_formula_weight         204.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2bc 2a'
_space_group_name_H-M_alt        'P m n b'
_symmetry_space_group_name_Hall  '-P 2bc 2a'
_symmetry_space_group_name_H-M   'P m n b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                   7.1767(3)
_cell_length_b                   7.3661(4)
_cell_length_c                   12.3418(7)
_cell_measurement_reflns_used    904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     652.44(6)
_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    'olex2.solve (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       ω
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.030886
_diffrn_orient_matrix_UB_12      -0.023129
_diffrn_orient_matrix_UB_13      0.077795
_diffrn_orient_matrix_UB_21      0.082449
_diffrn_orient_matrix_UB_22      -0.109437
_diffrn_orient_matrix_UB_23      -0.000521
_diffrn_orient_matrix_UB_31      0.107999
_diffrn_orient_matrix_UB_32      0.076932
_diffrn_orient_matrix_UB_33      0.022646
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_number            9265
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.321
_exptl_absorpt_correction_T_max  1.048
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.181
_refine_diff_density_min         -1.734
_refine_diff_density_rms         0.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0496
_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)+(0.1125P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                604
_reflns_number_total             814
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;

    shelx.res created by SHELXL-2014/7

TITL
CELL 0.71073 7.1767 7.3661 12.3418 90 90 90
ZERR 4 0.0003 0.0004 0.0007 0 0 0
LATT 1
SYMM -X,0.5-Y,0.5+Z
SYMM 0.5+X,-Y,-Z
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cu N O
UNIT 4 28 4 12 20
 
L.S. 4
PLAN  20
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./shelx.hkl">
REM </olex2.extras>
 
WGHT    0.112500
FVAR       0.25555
CU1   3    0.750000    0.315435    0.375135    10.50000    0.01363    0.01509 =
         0.01598   -0.00168    0.00000    0.00000
O1    5    0.750000    0.034956    0.671665    10.50000    0.05111    0.02300 =
         0.01660    0.00334    0.00000    0.00000
O4    5    0.750000    0.580092    0.425457    10.50000    0.02596    0.01678 =
         0.01356   -0.00031    0.00000    0.00000
O3    5    0.750000    0.078559    0.497928    10.50000    0.04994    0.03389 =
         0.01675    0.00085    0.00000    0.00000
N1    4    0.750000    0.141118    0.593625    10.50000    0.02900    0.01724 =
         0.01853    0.00080    0.00000    0.00000
C1    1    0.750000    0.685070    0.344827    10.50000    0.02102    0.01534 =
         0.02313    0.00007    0.00000    0.00000
AFIX  43
H1    2    0.750000    0.809595    0.357252    10.50000   -1.20000
AFIX   0
N2    4    0.476676    0.314603    0.372188    11.00000    0.01426    0.01952 =
         0.02078   -0.00373    0.00273    0.00139
AFIX 137
H2A   2    0.436908    0.380036    0.316150    11.00000   -1.20000
H2B   2    0.433226    0.362375    0.433417    11.00000   -1.20000
H2C   2    0.435903    0.201022    0.365662    11.00000   -1.20000
AFIX   0
O5    5    0.750000    0.630666    0.249810    10.50000    0.02463    0.01533 =
         0.01272    0.00393    0.00000    0.00000
O2    5    0.750000    0.304144    0.607606    10.50000    0.12620    0.01376 =
         0.03906   -0.00197    0.00000    0.00000
HKLF 4
 
REM
REM R1 =  0.0496 for     604 Fo > 4sig(Fo)  and  0.0734 for all     814 data
REM     59 parameters refined using      0 restraints
 
END  
     
WGHT      0.1125      0.0000 

REM Highest difference peak  1.181,  deepest hole -1.734,  1-sigma level  0.386
Q1    1   0.2500  0.1787  0.3744  10.50000  0.05    1.18
Q2    1   0.7500  0.8022  0.4386  10.50000  0.05    0.84
Q3    1   0.7500  0.9153  0.4454  10.50000  0.05    0.76
Q4    1   0.7500  0.3253  0.5840  10.50000  0.05    0.70
Q5    1   0.7500 -0.1454  0.5382  10.50000  0.05    0.69
Q6    1   0.2500  0.2360  0.4621  10.50000  0.05    0.69
Q7    1   0.8528  0.8176  0.4830  11.00000  0.05    0.69
Q8    1   0.7500  0.6863  0.4791  10.50000  0.05    0.65
Q9    1   0.7500  0.5846  0.4553  10.50000  0.05    0.65
Q10   1   0.9190  0.8426  0.4278  11.00000  0.05    0.63
Q11   1   0.7500  0.3263  0.6720  10.50000  0.05    0.62
Q12   1   0.2500  0.3568  0.3318  10.50000  0.05    0.62
Q13   1   0.3670  0.2004  0.4385  11.00000  0.05    0.61
Q14   1   0.9069 -0.0002  0.6101  11.00000  0.05    0.59
Q15   1   0.8995  0.3197  0.7211  11.00000  0.05    0.59
Q16   1   0.7500 -0.1307  0.7046  10.50000  0.05    0.57
Q17   1   0.8821  0.7243  0.4301  11.00000  0.05    0.55
Q18   1   0.3458  0.1869  0.3111  11.00000  0.05    0.55
Q19   1   0.7500  0.4184  0.7088  10.50000  0.05    0.54
Q20   1   0.4016  0.3225  0.2097  11.00000  0.05    0.54

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0496 for 604 Fo > 4sig(Fo) and 0.0734 for all 916 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.18, deepest hole -1.73
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0734
  REM R1_gt = 0.0496
  REM wR_ref = 0.1872
  REM GOOF = 1.205
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 916
  REM Reflections_gt = 604
  REM Parameters = n/a
  REM Hole = -1.73
  REM Peak = 1.18
  REM Flack = n/a

  
;
_cod_data_source_file            c6ce01601d2.cif
_cod_data_source_block           CuFmNO3
_cod_depositor_comments
'Adding full bibliography for 7227816--7227818.cif.'
_cod_database_code               7227817
_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_original_sample_id CuFmNO3
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z'
'x-1/2, -y-1/2, z-1/2'
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 0.7500 0.31543(12) 0.37513(7) 0.0149(4) Uani 1 2 d S T P
O1 O 0.7500 0.0350(9) 0.6717(5) 0.0302(14) Uani 1 2 d S T P
O4 O 0.7500 0.5801(7) 0.4255(4) 0.0188(12) Uani 1 2 d S T P
O3 O 0.7500 0.0786(10) 0.4979(5) 0.0335(15) Uani 1 2 d S T P
N1 N 0.7500 0.1411(10) 0.5936(6) 0.0216(15) Uani 1 2 d S T P
C1 C 0.7500 0.6851(11) 0.3448(7) 0.0198(17) Uani 1 2 d S T P
H1 H 0.7500 0.8096 0.3573 0.024 Uiso 1 2 calc RS T P
N2 N 0.4767(7) 0.3146(6) 0.3722(3) 0.0182(11) Uani 1 1 d . . .
H2A H 0.4369 0.3800 0.3161 0.022 Uiso 1 1 calc GR . .
H2B H 0.4332 0.3624 0.4334 0.022 Uiso 1 1 calc GR . .
H2C H 0.4359 0.2010 0.3657 0.022 Uiso 1 1 calc GR . .
O5 O 0.7500 0.6307(8) 0.2498(4) 0.0176(12) Uani 1 2 d S T P
O2 O 0.7500 0.3041(9) 0.6076(6) 0.060(3) 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 0.0136(6) 0.0151(6) 0.0160(6) -0.0017(3) 0.000 0.000
O1 0.051(4) 0.023(3) 0.017(3) 0.003(3) 0.000 0.000
O4 0.026(3) 0.017(3) 0.014(3) 0.000(2) 0.000 0.000
O3 0.050(4) 0.034(4) 0.017(3) 0.001(3) 0.000 0.000
N1 0.029(4) 0.017(3) 0.019(3) 0.001(3) 0.000 0.000
C1 0.021(4) 0.015(4) 0.023(4) 0.000(3) 0.000 0.000
N2 0.014(2) 0.020(3) 0.021(3) -0.0037(17) 0.0027(17) 0.0014(17)
O5 0.025(3) 0.015(3) 0.013(3) 0.004(2) 0.000 0.000
O2 0.126(9) 0.014(4) 0.039(4) -0.002(3) 0.000 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'
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 O3 121.4(2) . .
O4 Cu1 O5 149.1(2) . 6_556
N2 Cu1 O4 90.49(12) . .
N2 Cu1 O4 90.49(12) 7_755 .
N2 Cu1 O3 90.56(12) 7_755 .
N2 Cu1 O3 90.56(12) . .
N2 Cu1 N2 177.8(2) . 7_755
N2 Cu1 O5 89.09(11) . 6_556
N2 Cu1 O5 89.09(11) 7_755 6_556
O5 Cu1 O3 89.5(2) 6_556 .
C1 O4 Cu1 110.2(5) . .
N1 O3 Cu1 109.7(6) . .
O1 N1 O3 119.6(7) . .
O2 N1 O1 120.9(8) . .
O2 N1 O3 119.5(8) . .
O4 C1 H1 118.4 . .
O5 C1 O4 123.3(7) . .
O5 C1 H1 118.4 . .
Cu1 N2 H2A 109.5 . .
Cu1 N2 H2B 109.5 . .
Cu1 N2 H2C 109.5 . .
H2A N2 H2B 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
C1 O5 Cu1 119.7(5) . 6_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 2.046(6) .
Cu1 O3 2.311(7) .
Cu1 N2 1.962(5) .
Cu1 N2 1.962(5) 7_755
Cu1 O5 2.057(5) 6_556
O1 N1 1.241(10) .
O4 C1 1.260(10) .
O3 N1 1.268(9) .
N1 O2 1.213(10) .
C1 H1 0.9300 .
C1 O5 1.239(10) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
O5 Cu1 2.057(5) 6_566
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 0.000(3) .
Cu1 O3 N1 O1 180.000(2) .
Cu1 O3 N1 O2 0.000(2) .
O4 C1 O5 Cu1 180.000(2) 6_566
