#------------------------------------------------------------------------------
#$Date: 2017-05-06 00:41:24 +0300 (Sat, 06 May 2017) $
#$Revision: 196316 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/40/1544031.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_1544031
loop_
_publ_author_name
'Wang, Yingxia'
'Cui, Hao'
'Wei, Zhang-Wen'
'Wang, Hai-Ping'
'Zhang, Li'
'Su, Cheng-Yong'
_publ_section_title
;
 Engineering catalytic coordination space in a chemically stable
 Ir-porphyrin MOF with a confinement effect inverting conventional Si-H
 insertion chemoselectivity.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              775
_journal_page_last               780
_journal_paper_doi               10.1039/c6sc03288e
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C144 H72 Cl3 Hf12 Ir3 N12 O64'
_chemical_formula_weight         5818.96
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-07 deposited with the CCDC.
2016-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.3207(2)
_cell_length_b                   38.3207(2)
_cell_length_c                   38.32070(2)
_cell_measurement_reflns_used    11933
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.7640
_cell_measurement_theta_min      3.4310
_cell_volume                     56273.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            18019
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        64.772
_diffrn_reflns_theta_max         64.772
_diffrn_reflns_theta_min         3.647
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    0.687
_exptl_crystal_description       Block
_exptl_crystal_F_000             10712
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.485
_refine_diff_density_min         -5.540
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         4361
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0991
_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)+(0.0912P)²+1988.9337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2464
_refine_ls_wR_factor_ref         0.2476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4146
_reflns_number_total             4361
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6sc03288e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;Adding full bibliography for 1544031.cif.

 Adding full bibliography for 1544031.cif.
;
_cod_original_cell_volume        56273.0(9)
_cod_database_code               1544031
_shelx_shelxl_version_number     2014/7
_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_min   0.603
_shelx_estimated_absorpt_t_max   0.603
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, y+1/2, z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'x+1/2, -y+1/2, z+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-z+1/2, x+1/2, y+1/2'
'y+1/2, -z+1/2, x+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, y+1/2, x+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
Hf1 Hf 0.27144(2) 0.20721(2) 0.20721(2) 0.0803(4) Uani 1 2 d DS T P
Ir1 Ir 0.5000 0.2500 0.0000 0.1274(11) Uani 1 8 d S TU P
Cl1 Cl 0.5000 0.3143(11) 0.0000 0.28(2) Uani 0.5 4 d S TU P
O1 O 0.3155(2) 0.2224(3) 0.1721(2) 0.086(3) Uani 1 1 d D U .
O2 O 0.3056(4) 0.2422(3) 0.2422(3) 0.109(5) Uani 1 2 d DS TU P
O3 O 0.2496(3) 0.1957(5) 0.1528(3) 0.170(6) Uani 1 1 d D U .
O4 O 0.2144(3) 0.2144(3) 0.2144(3) 0.061(4) Uani 1 6 d DS TU P
N1 N 0.5000 0.2479(3) 0.0522(2) 0.059(3) Uani 1 2 d S TU P
C1 C 0.4712(3) 0.2468(3) 0.0724(3) 0.069(3) Uani 1 1 d . U .
C2 C 0.4814(3) 0.2443(4) 0.1087(3) 0.091(4) Uani 1 1 d . U .
H2 H 0.4665 0.2429 0.1284 0.109 Uiso 1 1 calc R U .
C3 C 0.4373(2) 0.2500 0.0627(2) 0.059(4) Uani 1 2 d S TU P
C4 C 0.4093(4) 0.2500 0.0907(4) 0.085(5) Uani 1 2 d S TU P
C5 C 0.4028(4) 0.2791(5) 0.1088(4) 0.107(5) Uani 1 1 d . U .
H5 H 0.4163 0.2994 0.1045 0.128 Uiso 1 1 calc R U .
C6 C 0.3764(4) 0.2798(4) 0.1339(4) 0.090(4) Uani 1 1 d . U .
H6 H 0.3709 0.3009 0.1457 0.108 Uiso 1 1 calc R U .
C7 C 0.3587(3) 0.2500 0.1413(3) 0.075(5) Uani 1 2 d S TU P
C8 C 0.3303(4) 0.2500 0.1697(4) 0.083(5) Uani 1 2 d S TU 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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -6.1794 4.9776 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 '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
O2 Hf1 O2 112.5(8) 84 83
O2 Hf1 O4 70.4(4) 84 .
O2 Hf1 O4 70.4(4) 83 .
O2 Hf1 O1 144.8(4) 84 70
O2 Hf1 O1 78.6(4) 83 70
O4 Hf1 O1 141.8(3) . 70
O2 Hf1 O1 78.6(4) 84 .
O2 Hf1 O1 144.8(4) 83 .
O4 Hf1 O1 141.8(3) . .
O1 Hf1 O1 75.2(5) 70 .
O2 Hf1 O3 135.7(5) 84 70
O2 Hf1 O3 82.6(6) 83 70
O4 Hf1 O3 77.1(5) . 70
O1 Hf1 O3 77.2(4) 70 70
O1 Hf1 O3 113.4(5) . 70
O2 Hf1 O3 82.6(6) 84 .
O2 Hf1 O3 135.7(5) 83 .
O4 Hf1 O3 77.1(5) . .
O1 Hf1 O3 113.4(5) 70 .
O1 Hf1 O3 77.2(4) . .
O3 Hf1 O3 61.1(8) 70 .
O2 Hf1 O2 74.7(5) 84 .
O2 Hf1 O2 74.7(5) 83 .
O4 Hf1 O2 114.6(6) . .
O1 Hf1 O2 76.6(4) 70 .
O1 Hf1 O2 76.6(4) . .
O3 Hf1 O2 148.1(4) 70 .
O3 Hf1 O2 148.1(4) . .
O2 Hf1 Hf1 93.6(4) 84 83
O2 Hf1 Hf1 39.8(4) 83 83
O4 Hf1 Hf1 94.9(4) . 83
O1 Hf1 Hf1 73.6(3) 70 83
O1 Hf1 Hf1 109.2(3) . 83
O3 Hf1 Hf1 118.8(4) 70 83
O3 Hf1 Hf1 172.0(3) . 83
O2 Hf1 Hf1 35.0(2) . 83
O2 Hf1 Hf1 39.8(4) 84 84
O2 Hf1 Hf1 93.6(4) 83 84
O4 Hf1 Hf1 94.9(4) . 84
O1 Hf1 Hf1 109.2(3) 70 84
O1 Hf1 Hf1 73.6(3) . 84
O3 Hf1 Hf1 172.0(3) 70 84
O3 Hf1 Hf1 118.8(4) . 84
O2 Hf1 Hf1 35.0(2) . 84
Hf1 Hf1 Hf1 60.06(4) 83 84
O2 Hf1 Hf1 89.4(4) 84 12
O2 Hf1 Hf1 32.6(4) 83 12
O4 Hf1 Hf1 38.4(3) . 12
O1 Hf1 Hf1 110.4(2) 70 12
O1 Hf1 Hf1 163.6(3) . 12
O3 Hf1 Hf1 83.0(4) 70 12
O3 Hf1 Hf1 112.7(3) . 12
O2 Hf1 Hf1 89.5(3) . 12
Hf1 Hf1 Hf1 59.97(2) 83 12
Hf1 Hf1 Hf1 90.0 84 12
O2 Hf1 Hf1 32.6(4) 84 11
O2 Hf1 Hf1 89.4(4) 83 11
O4 Hf1 Hf1 38.4(3) . 11
O1 Hf1 Hf1 163.6(3) 70 11
O1 Hf1 Hf1 110.4(2) . 11
O3 Hf1 Hf1 112.7(3) 70 11
O3 Hf1 Hf1 83.0(4) . 11
O2 Hf1 Hf1 89.5(3) . 11
Hf1 Hf1 Hf1 90.0 83 11
Hf1 Hf1 Hf1 59.97(2) 84 11
Hf1 Hf1 Hf1 60.0 12 11
N1 Ir1 N1 175.5(8) 82 80_554
N1 Ir1 N1 90.09(3) 82 51
N1 Ir1 N1 90.09(3) 80_554 51
N1 Ir1 N1 90.09(3) 82 .
N1 Ir1 N1 90.09(3) 80_554 .
N1 Ir1 N1 175.5(8) 51 .
N1 Ir1 Cl1 87.7(4) 82 .
N1 Ir1 Cl1 87.7(4) 80_554 .
N1 Ir1 Cl1 92.3(4) 51 .
N1 Ir1 Cl1 92.3(4) . .
N1 Ir1 Cl1 92.3(4) 82 80_554
N1 Ir1 Cl1 92.3(4) 80_554 80_554
N1 Ir1 Cl1 87.7(4) 51 80_554
N1 Ir1 Cl1 87.7(4) . 80_554
Cl1 Ir1 Cl1 180.0 . 80_554
C8 O1 Hf1 129.1(11) . .
Hf1 O2 Hf1 114.7(7) 83 84
Hf1 O2 Hf1 105.3(5) 83 .
Hf1 O2 Hf1 105.3(5) 84 .
Hf1 O4 Hf1 103.2(5) . 12
Hf1 O4 Hf1 103.2(5) . 11
Hf1 O4 Hf1 103.2(5) 12 11
C1 N1 C1 109.7(11) 54_655 .
C1 N1 Ir1 125.2(6) 54_655 .
C1 N1 Ir1 125.2(6) . .
N1 C1 C3 128.5(10) . .
N1 C1 C2 109.5(9) . .
C3 C1 C2 121.8(10) . .
C2 C2 C1 105.6(6) 54_655 .
C2 C2 H2 127.2 54_655 .
C1 C2 H2 127.2 . .
C1 C3 C1 122.1(13) 48 .
C1 C3 C4 118.9(6) 48 .
C1 C3 C4 118.9(6) . .
C5 C4 C5 120(2) . 48
C5 C4 C3 119.8(10) . .
C5 C4 C3 119.8(10) 48 .
C4 C5 C6 120.4(17) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
C7 C6 C5 119.3(15) . .
C7 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
C6 C7 C6 119.8(17) 48 .
C6 C7 C8 120.1(8) 48 .
C6 C7 C8 120.1(8) . .
O1 C8 O1 134(2) 48 .
O1 C8 C7 112.8(10) 48 .
O1 C8 C7 112.8(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hf1 O2 2.067(8) 84
Hf1 O2 2.067(8) 83
Hf1 O4 2.221(8) .
Hf1 O1 2.234(8) 70
Hf1 O1 2.234(8) .
Hf1 O3 2.290(13) 70
Hf1 O3 2.290(13) .
Hf1 O2 2.305(14) .
Hf1 Hf1 3.478(2) 83
Hf1 Hf1 3.478(2) 84
Hf1 Hf1 3.4810(11) 12
Hf1 Hf1 3.4810(11) 11
Ir1 N1 2.001(10) 82
Ir1 N1 2.001(10) 80_554
Ir1 N1 2.001(10) 51
Ir1 N1 2.001(10) .
Ir1 Cl1 2.47(4) .
Ir1 Cl1 2.47(4) 80_554
O1 C8 1.202(11) .
O2 Hf1 2.067(8) 83
O2 Hf1 2.067(8) 84
O4 Hf1 2.221(8) 12
O4 Hf1 2.221(8) 11
N1 C1 1.348(11) 54_655
N1 C1 1.348(11) .
C1 C3 1.359(12) .
C1 C2 1.449(16) .
C2 C2 1.42(3) 54_655
C2 H2 0.9500 .
C3 C1 1.359(12) 48
C3 C4 1.52(2) .
C4 C5 1.333(18) .
C4 C5 1.333(18) 48
C5 C6 1.399(18) .
C5 H5 0.9500 .
C6 C7 1.357(16) .
C6 H6 0.9500 .
C7 C6 1.357(16) 48
C7 C8 1.54(2) .
C8 O1 1.202(11) 48
