#------------------------------------------------------------------------------
#$Date: 2019-03-01 01:27:00 +0200 (Fri, 01 Mar 2019) $
#$Revision: 213903 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/06/1550666.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_1550666
loop_
_publ_author_name
'Kong, Xiang-Jing'
'He, Tao'
'Zhang, Yongzheng'
'Wu, Xue-Qian'
'Wang, Si-Nan'
'Xu, Ming-Ming'
'Si, Guang-Rui'
'Li, Jian-Rong Jeff'
_publ_section_title
;
 Constructing New Metal-Organic Frameworks with Complicated Ligands
 Generated from “One-Pot” In Situ Reactions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00178F
_journal_year                    2019
_chemical_formula_moiety         '0.06(C252 H162 Cu18 N18 O72)'
_chemical_formula_sum            'C14 H9 Cu N O4'
_chemical_formula_weight         318.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-11-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-01-04 deposited with the CCDC.    2019-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   18.6355(7)
_cell_length_b                   18.6355(7)
_cell_length_c                   34.4019(12)
_cell_measurement_reflns_used    3995
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      74.2420
_cell_measurement_theta_min      3.7200
_cell_volume                     10346.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  20.00   1.00    3.00    --  -41.94  57.00 -90.00   90
  2  ω      6.00  36.00   1.00    3.00    --   41.94 -38.00 -60.00   30
  3  ω    145.00 175.00   1.00   10.00    --  107.13 125.00 -60.00   30
  4  ω     84.00 177.00   1.00   10.00    --  107.13  45.00 120.00   93
  5  ω     95.00 157.00   1.00   10.00    --  107.13 125.00 120.00   62
  6  ω     36.00 104.00   1.00   10.00    --  107.13 -61.00  60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0066536000
_diffrn_orient_matrix_UB_12      0.0013675000
_diffrn_orient_matrix_UB_13      -0.0446060000
_diffrn_orient_matrix_UB_21      -0.0942962000
_diffrn_orient_matrix_UB_22      -0.0355188000
_diffrn_orient_matrix_UB_23      -0.0032414000
_diffrn_orient_matrix_UB_31      0.0134318000
_diffrn_orient_matrix_UB_32      0.0886175000
_diffrn_orient_matrix_UB_33      -0.0006567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            7625
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.756
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    0.921
_exptl_crystal_description       block
_exptl_crystal_F_000             2898
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0750P)²+16.2290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2064
_reflns_number_total             2276
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-101(Cu)
_cod_original_cell_volume        10346.5(9)
_cod_database_code               1550666
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O N Cu'
_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.
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Others
 Fixed Sof: H00A(0.5) H00B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 N004(H00A,H00B)
3.b Aromatic/amide H refined with riding coordinates:
 C007(H007), C00A(H00C), C00C(H00D), C00D(H00E)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.799
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
Cu01 Cu 1.14330(2) 0.85670(2) 0.30179(2) 0.02064(18) Uani 1 2 d S T P
O002 O 1.07712(10) 0.77466(11) 0.38306(4) 0.0379(4) Uani 1 1 d . . .
O003 O 1.03815(10) 0.81507(11) 0.32974(4) 0.0390(4) Uani 1 1 d . . .
N004 N 0.76862(8) 0.53723(16) 0.58431(6) 0.0348(6) Uani 1 2 d S T P
H00A H 0.7909 0.5047 0.5857 0.042 Uiso 0.5 1 calc R . .
H00B H 0.7139 0.5047 0.5857 0.042 Uiso 0.5 1 calc R . .
C005 C 0.83015(11) 0.6603(2) 0.47556(8) 0.0335(7) Uani 1 2 d S T P
C006 C 1.02690(14) 0.78571(14) 0.36374(6) 0.0308(5) Uani 1 1 d . . .
C007 C 0.89028(11) 0.7806(2) 0.36387(8) 0.0344(7) Uani 1 2 d S T P
H007 H 0.9026 0.8052 0.3394 0.041 Uiso 1 2 calc RS T P
C008 C 0.94554(14) 0.76209(15) 0.38220(6) 0.0347(5) Uani 1 1 d . . .
C009 C 0.78875(9) 0.57750(19) 0.54751(8) 0.0325(7) Uani 1 2 d S T P
C00A C 0.92613(15) 0.72405(16) 0.41853(6) 0.0379(5) Uani 1 1 d . . .
H00C H 0.9639 0.7126 0.4307 0.045 Uiso 1 1 calc R . .
C00B C 0.85130(11) 0.7026(2) 0.43733(9) 0.0356(7) Uani 1 2 d S T P
C00C C 0.7363(2) 0.5979(3) 0.52972(8) 0.0688(10) Uani 1 1 d . . .
H00D H 0.6859 0.5842 0.5413 0.083 Uiso 1 1 calc R . .
C00D C 0.7579(2) 0.6393(3) 0.49419(9) 0.0725(11) Uani 1 1 d . . .
H00E H 0.7213 0.6531 0.4827 0.087 Uiso 1 1 calc R . .
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'
H H 0.0000 0.0000 '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'
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
O002 Cu01 Cu01 84.12(4) 31_765 31_765
O002 Cu01 Cu01 84.12(4) 16_545 31_765
O002 Cu01 O002 89.22(11) 16_545 31_765
O002 Cu01 N004 97.69(6) 16_545 15_664
O002 Cu01 N004 97.69(6) 31_765 15_664
O003 Cu01 Cu01 84.01(4) . 31_765
O003 Cu01 Cu01 84.01(4) 22_775 31_765
O003 Cu01 O002 89.95(8) . 16_545
O003 Cu01 O002 168.13(6) . 31_765
O003 Cu01 O002 89.95(8) 22_775 31_765
O003 Cu01 O002 168.13(6) 22_775 16_545
O003 Cu01 O003 88.43(11) . 22_775
O003 Cu01 N004 94.16(6) . 15_664
O003 Cu01 N004 94.16(6) 22_775 15_664
N004 Cu01 Cu01 177.44(7) 15_664 31_765
C006 O002 Cu01 122.79(13) . 31_765
C006 O003 Cu01 122.81(14) . .
Cu01 N004 H00A 108.4 8_655 .
Cu01 N004 H00B 108.4 8_655 .
H00A N004 H00B 107.5 . .
C009 N004 Cu01 115.46(19) . 8_655
C009 N004 H00A 108.4 . .
C009 N004 H00B 108.4 . .
C00D C005 C00B 122.21(15) 23_655 .
C00D C005 C00B 122.21(15) . .
C00D C005 C00D 115.6(3) . 23_655
O002 C006 O003 126.1(2) . .
O002 C006 C008 117.42(17) . .
O003 C006 C008 116.46(18) . .
C008 C007 H007 120.1 23_655 .
C008 C007 H007 120.1 . .
C008 C007 C008 119.8(3) . 23_655
C007 C008 C006 120.21(19) . .
C007 C008 C00A 119.8(2) . .
C00A C008 C006 119.93(19) . .
C00C C009 N004 120.76(15) . .
C00C C009 N004 120.76(15) 23_655 .
C00C C009 C00C 118.5(3) . 23_655
C008 C00A H00C 119.1 . .
C008 C00A C00B 121.8(2) . .
C00B C00A H00C 119.1 . .
C00A C00B C005 121.55(14) 23_655 .
C00A C00B C005 121.56(14) . .
C00A C00B C00A 116.9(3) 23_655 .
C009 C00C H00D 120.0 . .
C009 C00C C00D 120.1(3) . .
C00D C00C H00D 120.0 . .
C005 C00D C00C 122.9(3) . .
C005 C00D H00E 118.6 . .
C00C C00D H00E 118.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu01 Cu01 2.6433(7) 31_765
Cu01 O002 1.9665(15) 31_765
Cu01 O002 1.9665(15) 16_545
Cu01 O003 1.9612(15) 22_775
Cu01 O003 1.9611(15) .
Cu01 N004 2.199(2) 15_664
O002 Cu01 1.9665(15) 31_765
O002 C006 1.246(3) .
O003 C006 1.264(3) .
N004 Cu01 2.199(2) 8_655
N004 H00A 0.8900 .
N004 H00B 0.8900 .
N004 C009 1.423(4) .
C005 C00B 1.482(4) .
C005 C00D 1.360(3) .
C005 C00D 1.360(3) 23_655
C006 C008 1.493(3) .
C007 H007 0.9300 .
C007 C008 1.390(3) .
C007 C008 1.390(3) 23_655
C008 C00A 1.392(3) .
C009 C00C 1.359(3) .
C009 C00C 1.359(3) 23_655
C00A H00C 0.9300 .
C00A C00B 1.402(3) .
C00B C00A 1.402(3) 23_655
C00C H00D 0.9300 .
C00C C00D 1.393(4) .
C00D H00E 0.9300 .
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
1 -0.146 -0.289 -0.021 5998.0 1835.2
