#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:22:24 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229078 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/01/7230120.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_7230120
loop_
_publ_author_name
'Scott, Hayley S.'
'Mukherjee, Soumya'
'Turner, David R.'
'Polson, Matthew I. J.'
'Zaworotko, Michael J.'
'Kruger, Paul E.'
_publ_section_title
;
 Crystal engineering of dichromate pillared hybrid ultramicroporous
 materials incorporating pyrazole-based ligands
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1193
_journal_paper_doi               10.1039/C8CE00149A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C20 H22 Cr2 Cu N6 O7'
_chemical_formula_sum            'C20 H22 Cr2 Cu N6 O7'
_chemical_formula_weight         625.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-01-10 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.47(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.710(3)
_cell_length_b                   14.320(3)
_cell_length_c                   15.800(3)
_cell_measurement_reflns_used    36754
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      1.393
_cell_volume                     3307.0(12)
_computing_cell_refinement       XDS
_computing_data_collection       BluICE
_computing_data_reduction        XDS
_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      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Australian Synchrotron'
_diffrn_measurement_method       'scans in phi'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36754
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.393
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XSCALE in XDS'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7598
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0517
_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)+(0.0637P)²+3.3087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6898
_reflns_number_total             7598
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00149a2.cif
_cod_data_source_block           DICRO7Cu
_cod_depositor_comments
'Adding full bibliography for 7230120--7230121.cif.'
_cod_database_code               7230120
_shelxl_version_number           2014/6
_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.
;
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: Cr2A(0.5) O6A(0.5) Cr2(0.5) O6(0.5) O5A(0.5) O5(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), N6(H6), C12(H12), N3(H3), C11(H11), C1(H1), C2(H2),
 C4(H4), C5(H5)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_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, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.25062(2) 0.38463(2) 0.27017(2) 0.02915(11) Uani 1 1 d . . . . .
Cr1 Cr 0.16761(3) 0.29652(4) 0.04336(3) 0.04417(14) Uani 1 1 d . . . . .
O1 O 0.21735(14) 0.33803(15) 0.13194(13) 0.0402(4) Uani 1 1 d . . . . .
N4 N 0.16396(15) 0.49370(16) 0.24321(16) 0.0366(5) Uani 1 1 d . . . . .
C15 C 0.08222(19) 0.4819(2) 0.1957(2) 0.0412(6) Uani 1 1 d . . . . .
H15 H 0.0662 0.4216 0.1739 0.049 Uiso 1 1 calc R . . . .
O3 O 0.1635(3) 0.3761(2) -0.02984(18) 0.0748(9) Uani 1 1 d . . . . .
N5 N -0.14624(15) 0.81149(15) 0.18958(15) 0.0318(4) Uani 1 1 d . . . . .
C14 C 0.02161(19) 0.5542(2) 0.1781(2) 0.0422(6) Uani 1 1 d . . . . .
H14 H -0.0355 0.5432 0.1451 0.051 Uiso 1 1 calc R . . . .
O2 O 0.06791(18) 0.2595(3) 0.0565(2) 0.0831(10) Uani 1 1 d . . . . .
N6 N -0.07923(16) 0.85736(17) 0.15286(16) 0.0376(5) Uani 1 1 d . . . . .
H6 H -0.0857 0.9139 0.1312 0.045 Uiso 1 1 calc R . . . .
C13 C 0.04392(19) 0.6443(2) 0.2088(2) 0.0413(6) Uani 1 1 d . . . . .
O4 O 0.23798(16) 0.20405(15) 0.00938(14) 0.0450(5) Uani 1 1 d . . . . .
N1 N 0.35295(14) 0.46728(15) 0.23939(15) 0.0312(4) Uani 1 1 d . . . . .
C12 C 0.1287(2) 0.6561(2) 0.2562(2) 0.0483(7) Uani 1 1 d . . . . .
H12 H 0.1469 0.7162 0.2772 0.058 Uiso 1 1 calc R . . . .
N3 N 0.66072(16) 0.73844(16) 0.11864(15) 0.0357(5) Uani 1 1 d D . . . .
H3 H 0.6959 0.7560 0.0800 0.043 Uiso 1 1 calc DR . . . .
C11 C 0.1867(2) 0.5802(2) 0.2730(2) 0.0450(7) Uani 1 1 d . . . . .
H11 H 0.2439 0.5893 0.3062 0.054 Uiso 1 1 calc R . . . .
N2 N 0.66002(15) 0.78088(15) 0.19578(15) 0.0325(4) Uani 1 1 d . . . . .
C16 C -0.01958(19) 0.7228(2) 0.1919(2) 0.0382(6) Uani 1 1 d . . . . .
C19 C -0.11039(17) 0.72770(18) 0.21282(17) 0.0326(5) Uani 1 1 d . . . . .
C17 C -0.0028(2) 0.8067(2) 0.1536(2) 0.0424(6) Uani 1 1 d . . . . .
C20 C -0.1625(2) 0.6536(2) 0.2530(2) 0.0410(6) Uani 1 1 d . . . . .
H20A H -0.2094 0.6826 0.2837 0.062 Uiso 1 1 calc GR . . . .
H20B H -0.1206 0.6173 0.2929 0.062 Uiso 1 1 calc GR . . . .
H20C H -0.1919 0.6121 0.2087 0.062 Uiso 1 1 calc GR . . . .
C18 C 0.0786(2) 0.8413(3) 0.1136(3) 0.0648(11) Uani 1 1 d . . . . .
H18A H 0.0989 0.9010 0.1394 0.097 Uiso 1 1 calc GR . . . .
H18B H 0.0618 0.8498 0.0523 0.097 Uiso 1 1 calc GR . . . .
H18C H 0.1283 0.7956 0.1230 0.097 Uiso 1 1 calc GR . . . .
C1 C 0.34837(19) 0.50897(19) 0.16290(18) 0.0362(5) Uani 1 1 d . . . . .
H1 H 0.2980 0.4953 0.1217 0.043 Uiso 1 1 calc R . . . .
C2 C 0.41462(19) 0.5715(2) 0.14165(18) 0.0377(6) Uani 1 1 d . . . . .
H2 H 0.4096 0.5991 0.0867 0.045 Uiso 1 1 calc R . . . .
C3 C 0.48900(18) 0.59338(19) 0.20211(17) 0.0339(5) Uani 1 1 d . . . . .
C4 C 0.49382(18) 0.5489(2) 0.28137(18) 0.0364(5) Uani 1 1 d . . . . .
H4 H 0.5436 0.5608 0.3237 0.044 Uiso 1 1 calc R . . . .
C5 C 0.42509(18) 0.48719(19) 0.29751(18) 0.0355(5) Uani 1 1 d . . . . .
H5 H 0.4288 0.4577 0.3517 0.043 Uiso 1 1 calc R . . . .
C6 C 0.55946(18) 0.66129(19) 0.18284(18) 0.0354(5) Uani 1 1 d . . . . .
C7 C 0.59835(18) 0.73363(19) 0.23567(17) 0.0334(5) Uani 1 1 d . . . . .
C9 C 0.6015(2) 0.6667(2) 0.10823(19) 0.0384(6) Uani 1 1 d . . . . .
C8 C 0.5774(2) 0.7600(2) 0.32280(19) 0.0424(6) Uani 1 1 d . . . . .
H8A H 0.6224 0.7314 0.3654 0.064 Uiso 1 1 calc GR . . . .
H8B H 0.5160 0.7379 0.3313 0.064 Uiso 1 1 calc GR . . . .
H8C H 0.5799 0.8281 0.3289 0.064 Uiso 1 1 calc GR . . . .
C10 C 0.5908(3) 0.6098(2) 0.0285(2) 0.0511(8) Uani 1 1 d . . . . .
H10A H 0.5396 0.6342 -0.0103 0.077 Uiso 1 1 calc GR . . . .
H10B H 0.5787 0.5447 0.0425 0.077 Uiso 1 1 calc GR . . . .
H10C H 0.6472 0.6133 0.0010 0.077 Uiso 1 1 calc GR . . . .
Cr2A Cr 0.23857(13) 0.0828(2) 0.0140(2) 0.0340(4) Uani 0.5 1 d . . P A 2
O7 O 0.2714(2) 0.04888(17) -0.07920(16) 0.0588(7) Uani 1 1 d . . . . .
O6A O 0.2890(5) 0.0409(5) 0.0982(4) 0.0621(16) Uani 0.5 1 d . . P A 2
Cr2 Cr 0.2664(2) 0.0786(3) 0.0100(2) 0.0711(9) Uani 0.5 1 d . . P A 1
O6 O 0.3413(9) 0.0590(7) 0.0742(7) 0.129(4) Uani 0.5 1 d . U P A 1
O5A O 0.1330(4) 0.0427(4) 0.0063(4) 0.0628(15) Uani 0.5 1 d . . P A 2
O5 O 0.1824(9) 0.0273(6) 0.0538(6) 0.113(3) Uani 0.5 1 d . U P A 1
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'
Cr Cr 0.3209 0.6236 '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
O1 Cu1 O7 172.85(9) . 4_566
N4 Cu1 O1 87.85(9) . .
N4 Cu1 O7 85.12(10) . 4_566
N5 Cu1 O1 93.50(9) 2_545 .
N5 Cu1 N4 89.05(9) 2_545 .
N5 Cu1 O7 85.13(9) 2_545 4_566
N1 Cu1 O1 91.50(9) . .
N1 Cu1 N4 88.05(9) . .
N1 Cu1 N5 174.12(9) . 2_545
N1 Cu1 O7 89.53(9) . 4_566
N2 Cu1 O1 95.91(9) 2_645 .
N2 Cu1 N4 176.12(10) 2_645 .
N2 Cu1 N5 91.71(9) 2_645 2_545
N2 Cu1 N1 90.85(9) 2_645 .
N2 Cu1 O7 91.15(10) 2_645 4_566
O1 Cr1 O3 109.66(15) . .
O1 Cr1 O4 108.01(11) . .
O3 Cr1 O4 106.31(14) . .
O2 Cr1 O1 110.00(14) . .
O2 Cr1 O3 111.5(2) . .
O2 Cr1 O4 111.29(15) . .
Cr1 O1 Cu1 164.20(13) . .
C15 N4 Cu1 121.18(19) . .
C11 N4 Cu1 120.45(19) . .
C11 N4 C15 118.4(2) . .
N4 C15 H15 118.9 . .
N4 C15 C14 122.3(3) . .
C14 C15 H15 118.9 . .
N6 N5 Cu1 119.64(16) . 2
C19 N5 Cu1 131.71(18) . 2
C19 N5 N6 105.4(2) . .
C15 C14 H14 120.0 . .
C15 C14 C13 120.1(3) . .
C13 C14 H14 120.0 . .
N5 N6 H6 123.8 . .
C17 N6 N5 112.4(2) . .
C17 N6 H6 123.8 . .
C14 C13 C16 121.5(3) . .
C12 C13 C14 117.3(3) . .
C12 C13 C16 121.2(3) . .
Cr1 O4 Cr2 148.52(16) . .
Cr2A O4 Cr1 136.29(15) . .
C1 N1 Cu1 120.98(18) . .
C1 N1 C5 118.2(2) . .
C5 N1 Cu1 120.64(18) . .
C13 C12 H12 120.0 . .
C11 C12 C13 120.1(3) . .
C11 C12 H12 120.0 . .
N2 N3 H3 123.8 . .
C9 N3 H3 123.8 . .
C9 N3 N2 112.3(2) . .
N4 C11 C12 121.9(3) . .
N4 C11 H11 119.1 . .
C12 C11 H11 119.1 . .
N3 N2 Cu1 119.79(16) . 2_655
C7 N2 Cu1 134.42(19) . 2_655
C7 N2 N3 105.6(2) . .
C19 C16 C13 126.5(3) . .
C17 C16 C13 127.3(3) . .
C17 C16 C19 106.2(2) . .
N5 C19 C16 109.4(2) . .
N5 C19 C20 123.1(2) . .
C16 C19 C20 127.5(2) . .
N6 C17 C16 106.6(2) . .
N6 C17 C18 121.9(3) . .
C16 C17 C18 131.5(3) . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18B 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N1 C1 H1 118.7 . .
N1 C1 C2 122.5(3) . .
C2 C1 H1 118.7 . .
C1 C2 H2 120.2 . .
C1 C2 C3 119.5(3) . .
C3 C2 H2 120.2 . .
C2 C3 C6 121.2(2) . .
C4 C3 C2 117.6(2) . .
C4 C3 C6 121.2(2) . .
C3 C4 H4 120.3 . .
C5 C4 C3 119.3(3) . .
C5 C4 H4 120.3 . .
N1 C5 C4 122.8(3) . .
N1 C5 H5 118.6 . .
C4 C5 H5 118.6 . .
C7 C6 C3 127.5(2) . .
C9 C6 C3 126.8(2) . .
C9 C6 C7 105.7(2) . .
N2 C7 C6 110.0(2) . .
N2 C7 C8 121.7(2) . .
C6 C7 C8 128.3(2) . .
N3 C9 C6 106.4(2) . .
N3 C9 C10 121.7(3) . .
C6 C9 C10 132.0(3) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O7 Cr2A O4 104.69(19) . .
O6A Cr2A O4 114.7(3) . .
O6A Cr2A O7 118.7(3) . .
O6A Cr2A O5A 106.4(4) . .
O5A Cr2A O4 110.2(3) . .
O5A Cr2A O7 101.3(3) . .
O7 Cr2 O4 108.0(2) . .
O7 Cr2 O5 112.9(4) . .
O6 Cr2 O4 110.4(5) . .
O6 Cr2 O7 119.9(6) . .
O6 Cr2 O5 99.6(7) . .
O5 Cr2 O4 104.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 2.283(2) .
Cu1 N4 2.031(2) .
Cu1 N5 2.020(2) 2_545
Cu1 N1 2.017(2) .
Cu1 N2 2.016(2) 2_645
Cu1 O7 2.550(3) 4_566
Cr1 O1 1.618(2) .
Cr1 O3 1.619(3) .
Cr1 O2 1.595(3) .
Cr1 O4 1.800(2) .
N4 C15 1.354(4) .
N4 C11 1.354(4) .
C15 H15 0.9500 .
C15 C14 1.374(4) .
N5 Cu1 2.020(2) 2
N5 N6 1.367(3) .
N5 C19 1.345(3) .
C14 H14 0.9500 .
C14 C13 1.404(4) .
N6 H6 0.8800 .
N6 C17 1.336(4) .
C13 C12 1.391(4) .
C13 C16 1.467(4) .
O4 Cr2A 1.738(4) .
O4 Cr2 1.845(4) .
N1 C1 1.343(4) .
N1 C5 1.353(3) .
C12 H12 0.9500 .
C12 C11 1.388(4) .
N3 H3 0.8800 .
N3 N2 1.363(3) .
N3 C9 1.345(4) .
C11 H11 0.9500 .
N2 Cu1 2.016(2) 2_655
N2 C7 1.344(3) .
C16 C19 1.414(4) .
C16 C17 1.380(4) .
C19 C20 1.492(4) .
C17 C18 1.500(4) .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C1 H1 0.9500 .
C1 C2 1.392(4) .
C2 H2 0.9500 .
C2 C3 1.405(4) .
C3 C4 1.400(4) .
C3 C6 1.478(4) .
C4 H4 0.9500 .
C4 C5 1.387(4) .
C5 H5 0.9500 .
C6 C7 1.410(4) .
C6 C9 1.394(4) .
C7 C8 1.493(4) .
C9 C10 1.493(4) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
Cr2A O7 1.673(4) .
Cr2A O6A 1.567(7) .
Cr2A O5A 1.647(6) .
O7 Cr2 1.482(4) .
Cr2 O6 1.439(9) .
Cr2 O5 1.654(9) .
