#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:11:28 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229511 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/75/7047524.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_7047524
loop_
_publ_author_name
'Hassanpoor, Azam'
'Mirzaei, Masoud'
'Niknam Shahrak, Mahdi'
'Majcher, Anna M.'
_publ_section_title
;
 Developing a magnetic metal organic framework of copper bearing a mixed
 azido/butane-1,4-dicarboxylate bridge: magnetic and gas adsorption
 properties.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13849
_journal_page_last               13860
_journal_paper_doi               10.1039/c8dt02986e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.25(C12 H24 Cu4 N12 O12), 1[H2O]'
_chemical_formula_sum            'C3 H8 Cu N3 O4'
_chemical_formula_weight         213.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5356)
;
_audit_update_record
;
2018-09-07 deposited with the CCDC.
2018-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.469(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5619(4)
_cell_length_b                   6.4760(2)
_cell_length_c                   7.4973(2)
_cell_measurement_reflns_used    2919
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.0950
_cell_measurement_theta_min      6.0980
_cell_volume                     703.80(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    9.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798 -104.0000   29.0000 53

#__ type_ start__ end____ width___ exp.time_
  2 omega  -81.00    0.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  104.0000  130.0000 81

#__ type_ start__ end____ width___ exp.time_
  3 omega   51.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -104.0000   29.0000 53

#__ type_ start__ end____ width___ exp.time_
  4 omega  108.00  134.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  104.0000  130.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega -120.00  -92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000  150.0000 28

#__ type_ start__ end____ width___ exp.time_
  6 omega -122.00  -82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000  -60.0000 40

#__ type_ start__ end____ width___ exp.time_
  7 omega -122.00  -87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000 -120.0000 35

#__ type_ start__ end____ width___ exp.time_
  8 omega -125.00  -85.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000   60.0000 40

#__ type_ start__ end____ width___ exp.time_
  9 omega   39.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 10 omega   75.00  101.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 11 omega   82.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 57

#__ type_ start__ end____ width___ exp.time_
 12 omega   58.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  150.0000 40

#__ type_ start__ end____ width___ exp.time_
 13 omega   41.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 69

#__ type_ start__ end____ width___ exp.time_
 14 omega  145.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 33

#__ type_ start__ end____ width___ exp.time_
 15 omega   39.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 52

#__ type_ start__ end____ width___ exp.time_
 16 omega   40.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   60.0000 33

#__ type_ start__ end____ width___ exp.time_
 17 omega   97.00  144.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   60.0000 47

#__ type_ start__ end____ width___ exp.time_
 18 omega   53.00   79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega  108.00  174.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 66

#__ type_ start__ end____ width___ exp.time_
 20 omega -118.00   -9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  -77.0000  150.0000 109

#__ type_ start__ end____ width___ exp.time_
 21 omega -116.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -61.0000   60.0000 102

#__ type_ start__ end____ width___ exp.time_
 22 omega -120.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -77.0000  -30.0000 109

#__ type_ start__ end____ width___ exp.time_
 23 omega -116.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -61.0000 -150.0000 102

#__ type_ start__ end____ width___ exp.time_
 24 omega   82.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 96

#__ type_ start__ end____ width___ exp.time_
 25 omega   28.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 81

#__ type_ start__ end____ width___ exp.time_
 26 omega   83.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   90.0000 95

#__ type_ start__ end____ width___ exp.time_
 27 omega   38.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 60

#__ type_ start__ end____ width___ exp.time_
 28 omega   78.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 100

#__ type_ start__ end____ width___ exp.time_
 29 omega   82.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 68

#__ type_ start__ end____ width___ exp.time_
 30 omega   58.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000    0.0000 120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3958
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.260
_diffrn_reflns_theta_min         6.106
_exptl_absorpt_coefficient_mu    4.251
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_description       rod
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.1282
_exptl_crystal_size_mid          0.1004
_exptl_crystal_size_min          0.0706
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         794
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0242
_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)+(0.0406P)²+1.1121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                773
_reflns_number_total             794
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt02986e2.cif
_cod_data_source_block           ah81w
_cod_depositor_comments          'Adding full bibliography for 7047524.cif.'
_cod_database_code               7047524
_shelx_shelxl_version_number     2018/3
_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,H) groups
2. Restrained distances
 O2-H2C
 0.84 with sigma of 0.01
 O2-H2D
 0.84 with sigma of 0.01
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H3A(0.5) H3B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 36 electrons were 
found in a volume of 124Å^3 in 1 void. 
This is consistent with the presence of 
1[H2O] per formula unit 
which account for 40.0 electrons.
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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 0.250000 0.750000 1.000000 0.00873(15) Uani 1 2 d S T P
O1 O 0.35804(8) 0.82627(18) 0.87762(15) 0.0124(3) Uani 1 1 d . . .
N1 N 0.23156(14) 0.500000 0.8405(2) 0.0109(4) Uani 1 2 d S T P
N2 N 0.25733(13) 0.500000 0.6916(3) 0.0115(4) Uani 1 2 d S T P
N3 N 0.27983(18) 0.500000 0.5502(3) 0.0243(5) Uani 1 2 d S T P
C1 C 0.39220(16) 1.000000 0.8450(3) 0.0105(4) Uani 1 2 d S T P
C2 C 0.48023(16) 1.000000 0.7526(3) 0.0143(5) Uani 1 2 d S T P
H2A H 0.517297 0.876152 0.788715 0.017 Uiso 0.5 1 calc R . .
H2B H 0.517297 1.123848 0.788716 0.017 Uiso 0.5 1 calc R . .
C3 C 0.45648(16) 1.000000 0.5488(3) 0.0129(5) Uani 1 2 d S T P
H3A H 0.419132 0.876305 0.513504 0.015 Uiso 0.5 1 calc R . .
H3B H 0.419132 1.123695 0.513504 0.015 Uiso 0.5 1 calc R . .
O2 O 0.16001(12) 1.000000 0.8119(2) 0.0152(4) Uani 1 2 d DS T P
H2C H 0.172(3) 1.000000 0.704(2) 0.042(11) Uiso 1 2 d DS T P
H2D H 0.1018(7) 1.000000 0.794(7) 0.076(17) Uiso 1 2 d DS T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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 Cu1 O1 180.0 . 7_567
O1 Cu1 N1 90.45(6) 7_567 .
O1 Cu1 N1 90.45(6) . 7_567
O1 Cu1 N1 89.55(6) . .
O1 Cu1 N1 89.55(6) 7_567 7_567
O1 Cu1 O2 91.54(5) 7_567 .
O1 Cu1 O2 88.46(5) . .
N1 Cu1 N1 180.0 . 7_567
N1 Cu1 O2 81.02(5) 7_567 .
N1 Cu1 O2 98.98(5) . .
C1 O1 Cu1 131.60(12) . .
Cu1 N1 Cu1 106.90(8) . 4_547
N2 N1 Cu1 120.76(7) . 4_547
N2 N1 Cu1 120.76(7) . .
N3 N2 N1 178.7(2) . .
O1 C1 O1 125.9(2) 6_575 .
O1 C1 C2 117.05(10) . .
O1 C1 C2 117.04(10) 6_575 .
C1 C2 H2A 109.8 . .
C1 C2 H2B 109.8 . .
C1 C2 C3 109.59(19) . .
H2A C2 H2B 108.2 . .
C3 C2 H2A 109.8 . .
C3 C2 H2B 109.8 . .
C2 C3 H3A 109.4 . .
C2 C3 H3B 109.4 . .
C3 C3 C2 111.1(2) 5_676 .
C3 C3 H3A 109.4 5_676 .
C3 C3 H3B 109.4 5_676 .
H3A C3 H3B 108.0 . .
Cu1 O2 H2C 114(2) . .
Cu1 O2 H2D 124(2) . .
H2C O2 H2D 98(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9587(11) .
Cu1 O1 1.9587(11) 7_567
Cu1 N1 2.0154(11) .
Cu1 N1 2.0154(11) 7_567
Cu1 O2 2.4443(13) .
O1 C1 1.2634(15) .
N1 N2 1.211(3) .
N2 N3 1.139(3) .
C1 C2 1.514(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C2 C3 1.534(3) .
C3 C3 1.523(4) 5_676
C3 H3A 0.9900 .
C3 H3B 0.9900 .
O2 H2C 0.840(10) .
O2 H2D 0.845(10) .
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_1
_geom_torsion_site_symmetry_4
Cu1 O1 C1 O1 -4.9(3) . 6_575
Cu1 O1 C1 C2 177.44(13) . .
O1 C1 C2 C3 88.96(17) . .
O1 C1 C2 C3 -88.96(17) 6_575 .
C1 C2 C3 C3 180.000(0) . 5_676
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.029 61.9 17.9 '1/2 water'
2 0.500 0.500 -0.814 61.9 17.9 '1/2 water'
