#------------------------------------------------------------------------------
#$Date: 2019-11-22 23:49:15 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231597 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/60/4346049.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_4346049
loop_
_publ_author_name
'Gonzalez, Miguel I.'
'Bloch, Eric D.'
'Mason, Jarad A.'
'Teat, Simon J.'
'Long, Jeffrey R.'
_publ_section_title
;
 Single-crystal-to-single-crystal metalation of a metal-organic framework:
 a route toward structurally well-defined catalysts.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2995
_journal_page_last               3005
_journal_paper_doi               10.1021/acs.inorgchem.5b00096
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '0.5(C123.84 H74.24 N20.64 O56 Zr12), 4(O)'
_chemical_formula_sum            'C61.92 H37.05 N10.32 O32 Zr6'
_chemical_formula_weight         1984.90
_chemical_name_common            Zr6O4(OH)4(bpydc)5.16
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.520(2)
_cell_length_b                   26.520(2)
_cell_length_c                   26.520(2)
_cell_measurement_reflns_used    5088
_cell_measurement_temperature    100(2)
_cell_volume                     18652(2)
_computing_cell_refinement       'Bruker SAINT v8.27b'
_computing_data_reduction        'Bruker SAINT v8.27b'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-2014
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14200
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.325
_diffrn_reflns_theta_min         1.330
_diffrn_source                   'micro focus sealed tube'
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.4534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0624 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9251.
The λ/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             3907
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0329
_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)+(0.0639P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                704
_reflns_number_total             866
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00096_si_001.cif
_cod_data_source_block           mig006_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        18652(4)
_cod_database_code               4346049
_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   0.986
_shelx_estimated_absorpt_t_min   0.986
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{N9, C9}
3. Rigid bond restraints
 O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3: within 2.5A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N9) = Uanis(C9)
5. Others
 Fixed Sof: O2B(0.08333) O1(0.43) C4(0.215) C5(0.215) C8(0.215) C9(0.215)
 H9(0.215) N9(0.215) C10(0.43) H10(0.25) O2A(0.08333) O3(0.07)
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C10(H10A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'
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
O2B O 0.4594(2) -0.0406(2) 0.0406(2) 0.008(2) Uani 0.5 6 d S T P . 2
O1 O 0.42693(14) 0.0000 0.13363(14) 0.0248(9) Uani 0.86 2 d S T P . 1
C4 C 0.38187(15) 0.0000 0.11813(15) 0.0320(15) Uani 0.86 4 d S T P . 1
C5 C 0.34212(15) 0.0000 0.15788(15) 0.0447(17) Uani 0.86 4 d S T P . .
C8 C 0.27027(16) 0.0000 0.22973(16) 0.058(2) Uani 0.86 4 d S T P . .
C9 C 0.31879(17) 0.0000 0.24422(18) 0.084(2) Uani 0.43 2 d S T P . 1
H9 H 0.3277 0.0000 0.2789 0.100 Uiso 0.43 2 calc RS T P . 1
N9 N 0.31879(17) 0.0000 0.24422(18) 0.084(2) Uani 0.43 2 d S T P . 2
C10 C 0.3547(2) 0.0000 0.2076(2) 0.0736(19) Uani 0.86 2 d S T P . .
H10 H 0.3893 0.0000 0.2170 0.088 Uiso 0.5 2 calc RS T P A 1
H10A H 0.3893 0.0000 0.2170 0.088 Uiso 0.62(8) 2 calc RS T P B 2
Zr1 Zr 0.5000 0.0000 0.09320(2) 0.0118(3) Uani 1 8 d S T P . .
O2A O 0.4465(2) -0.0535(2) 0.0535(2) 0.020(3) Uani 0.5 6 d S T P . 1
O3 O 0.4424(12) 0.0000 0.1516(10) 0.044(9) Uani 0.14 2 d S TU P . 2
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'
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'
Zr Zr -2.9673 0.5597 '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
Zr1 O2B Zr1 115.65(17) . 153
Zr1 O2B Zr1 115.65(17) . 173
Zr1 O2B Zr1 115.65(17) 153 173
C4 O1 Zr1 132.1(4) . .
O1 C4 O1 128.0(6) 166 .
O1 C4 C5 116.0(3) 166 .
O1 C4 C5 116.0(3) . .
C10 C5 C4 120.8(3) . .
C10 C5 C4 120.8(3) 166 .
C10 C5 C10 118.4(6) . 166
C9 C8 C8 118.4(3) 166 145
C9 C8 C8 118.4(3) . 145
C9 C8 C9 123.3(6) 166 .
N9 C8 C8 118.4(3) 166 145
N9 C8 C8 118.4(3) . 145
N9 C8 N9 123.3(6) 166 .
C8 C9 H9 121.1 . .
C8 C9 C10 117.8(5) . .
C10 C9 H9 121.1 . .
C8 N9 C10 117.8(5) . .
C5 C10 H10 119.3 . .
C5 C10 H10A 119.3 . .
C9 C10 C5 121.4(5) . .
C9 C10 H10 119.3 . .
N9 C10 C5 121.4(5) . .
N9 C10 H10A 119.3 . .
O2B Zr1 O2B 62.8(3) 100_655 2_655
O2B Zr1 O2B 95.0(5) 100_655 99
O2B Zr1 O2B 95.0(5) . 2_655
O2B Zr1 O2B 62.8(3) . 100_655
O2B Zr1 O2B 62.8(3) . 99
O2B Zr1 O2B 62.8(3) 99 2_655
O2B Zr1 O3 147.90(14) . 181
O2B Zr1 O3 96.6(5) . 182_545
O2B Zr1 O3 147.90(14) 100_655 .
O2B Zr1 O3 147.90(14) 100_655 181
O2B Zr1 O3 147.90(14) 99 182_545
O2B Zr1 O3 96.6(5) 99 181
O2B Zr1 O3 147.90(14) 2_655 .
O2B Zr1 O3 96.6(5) 2_655 181
O2B Zr1 O3 96.6(5) 100_655 182_545
O2B Zr1 O3 147.90(14) . 2_655
O2B Zr1 O3 147.90(14) 2_655 182_545
O2B Zr1 O3 96.6(5) 100_655 2_655
O2B Zr1 O3 96.6(5) 99 .
O2B Zr1 O3 147.90(14) 99 2_655
O2B Zr1 O3 96.6(5) 2_655 2_655
O2B Zr1 O3 96.6(5) . .
O1 Zr1 O1 76.45(9) . 181
O1 Zr1 O1 76.45(9) 2_655 182_545
O1 Zr1 O1 122.1(2) 181 182_545
O1 Zr1 O1 76.45(9) 181 2_655
O1 Zr1 O1 76.45(9) . 182_545
O1 Zr1 O1 122.1(2) . 2_655
O3 Zr1 O3 59.6(7) 181 2_655
O3 Zr1 O3 89.2(11) 2_655 .
O3 Zr1 O3 59.6(7) 182_545 .
O3 Zr1 O3 89.2(11) 181 182_545
O3 Zr1 O3 59.6(7) 2_655 182_545
O3 Zr1 O3 59.6(7) 181 .
Zr1 O2A Zr1 101.0(3) . 153
Zr1 O2A Zr1 101.0(3) 153 173
Zr1 O2A Zr1 101.0(3) . 173
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O2B Zr1 2.065(2) .
O2B Zr1 2.065(2) 153
O2B Zr1 2.065(2) 173
O1 C4 1.264(5) .
O1 Zr1 2.215(4) .
C4 O1 1.264(5) 166
C4 C5 1.491(8) .
C5 C10 1.360(6) .
C5 C10 1.360(6) 166
C8 C8 1.520(12) 145
C8 C9 1.343(5) .
C8 C9 1.343(5) 166
C8 N9 1.343(5) .
C8 N9 1.343(5) 166
C9 H9 0.9500 .
C9 C10 1.360(7) .
N9 C10 1.360(7) .
C10 H10 0.9500 .
C10 H10A 0.9500 .
Zr1 O2B 2.065(2) 2_655
Zr1 O2B 2.065(2) 100_655
Zr1 O2B 2.065(2) 99
Zr1 O1 2.215(4) 181
Zr1 O1 2.215(4) 2_655
Zr1 O1 2.215(4) 182_545
Zr1 O3 2.18(4) 2_655
Zr1 O3 2.18(4) .
Zr1 O3 2.18(4) 182_545
Zr1 O3 2.18(4) 181
O2A Zr1 2.266(4) 153
O2A Zr1 2.266(4) 173
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
O1 C4 C5 C10 180.000(0) 166 .
O1 C4 C5 C10 180.000(0) . 166
O1 C4 C5 C10 0.000(0) . .
O1 C4 C5 C10 0.000(0) 166 166
C4 C5 C10 C9 180.000(0) . .
C8 C8 C9 C10 180.000(0) 145 .
C8 C8 N9 C10 180.000(0) 145 .
C8 C9 C10 C5 0.000(0) . .
C8 N9 C10 C5 0.000(0) . .
C9 C8 C9 C10 0.000(0) 166 .
N9 C8 N9 C10 0.000(0) 166 .
C10 C5 C10 C9 0.000(0) 166 .
C10 C5 C10 N9 0.000(0) 166 .
Zr1 O1 C4 O1 0.0 . 166
Zr1 O1 C4 C5 180.0 . .
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 -0.623 -0.942 -0.570 12759.6 2549.9
