#------------------------------------------------------------------------------
#$Date: 2019-11-22 22:24:58 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231424 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/31/4003192.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_4003192
loop_
_publ_author_name
'McKellar, Scott C.'
'Sotelo, Jorge'
'Greenaway, Alex'
'Mowat, John P. S.'
'Kvam, Odin'
'Morrison, Carole A.'
'Wright, Paul A.'
'Moggach, Stephen A.'
_publ_section_title
;
 Pore Shape Modification of a Microporous Metal--Organic Framework Using
 High Pressure: Accessing a New Phase with Oversized Guest Molecules
;
_journal_issue                   2
_journal_name_full               'Chemistry of Materials'
_journal_page_first              466
_journal_paper_doi               10.1021/acs.chemmater.5b02891
_journal_volume                  28
_journal_year                    2016
_chemical_formula_moiety         'C12 H6 O6 Sc1'
_chemical_formula_sum            'C12 H6 O6 Sc'
_chemical_formula_weight         291.13
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      70
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             15-06-01
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   8.777(6)
_cell_length_b                   20.772(14)
_cell_length_c                   34.38(2)
_cell_measurement_reflns_used    1385
_cell_measurement_temperature    293
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     6268(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5358
_diffrn_reflns_theta_full        17.483
_diffrn_reflns_theta_max         23.311
_diffrn_reflns_theta_min         2.291
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9012
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1072
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.0003318
_refine_ls_shift/su_mean         0.0000468
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 5.11 4.60 1.38 -0.359 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1315
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1315
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                677
_reflns_number_total             1090
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.43
_oxford_diffrn_Wilson_scale      640.81
_oxford_refine_ls_r_factor_ref   0.1027
_oxford_refine_ls_scale          0.05328(2)
_oxford_reflns_number_all        1072
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ST3018_0m in Fddd'
_cod_data_source_file            cm5b02891_si_003.cif
_cod_data_source_block           pent_immersion
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C12 H6 O6 Sc1'
_cod_database_code               4003192
_iucr_refine_instruction_details_constraints
;
#
# Punched on 01/06/15 at 14:25:39
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT SC   (    1 ,X'S,U'S)  UNTIL O    (    2 ) 
CONT O    (    3 ,X'S,U'S) 
CONT C    (    1 ,X'S,U'S)  UNTIL C    (    5 ) 
CONT C    (    6 ,X'S,U'S)  UNTIL C    (    8 ) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 01/06/15 at 14:25:39
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(1) 
VIBR .0, 0.00200 = O(3) TO C(5) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(4,-1,4,0,0,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(4,-1,4,0,0,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(4,-1,4,0,0,1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00500 = C(3) TO C(2,-1,4,0,0,1) 
VIBR .0, 0.00200 = C(5) TO C(6) 
VIBR .0, 0.00500 = O(3,-3,1,0,0,1) TO O(3) 
VIBR .0, 0.00500 = C(6) TO O(3) 
VIBR .0, 0.00500 = C(6) TO O(3,-3,1,0,0,1) 
VIBR .0, 0.00200 = C(6) TO C(7,-3,1,0,0,1) 
VIBR .0, 0.00200 = C(6) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00200 = C(6) TO C(8,4,2,0,0,-1) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00500 = C(7,-3,1,0,0,1) TO C(5) 
VIBR .0, 0.00500 = C(8,-2,1,0,1,1) TO C(5) 
VIBR .0, 0.00500 = C(8,-2,1,0,1,1) TO C(7,-3,1,0,0,1) 
VIBR .0, 0.00500 = C(8,4,2,0,0,-1) TO C(5) 
VIBR .0, 0.00500 = C(8,4,2,0,0,-1) TO C(7,-3,1,0,0,1) 
VIBR .0, 0.00500 = C(8,4,2,0,0,-1) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(7) TO C(5) 
VIBR .0, 0.00500 = C(7) TO C(7,-3,1,0,0,1) 
VIBR .0, 0.00500 = C(7) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(7) TO C(8,4,2,0,0,-1) 
VIBR .0, 0.00200 = C(7) TO C(7,-2,1,0,1,1) 
VIBR .0, 0.00200 = C(7) TO C(8) 
VIBR .0, 0.00500 = C(7,-2,1,0,1,1) TO C(6) 
VIBR .0, 0.00500 = C(8) TO C(6) 
VIBR .0, 0.00500 = C(8) TO C(7,-2,1,0,1,1) 
VIBR .0, 0.00200 = C(8) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(7) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(6,4,2,0,0,-1) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(6,4,2,0,0,-1) TO C(7) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = O(1) TO C(1) 
U(IJ) .0, 0.08000 = O(2) TO C(1) 
U(IJ) .0, 0.04000 = O(3) TO C(5) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(4,-1,4,0,0,1) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(5) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO C(7,-3,1,0,0,1) 
U(IJ) .0, 0.04000 = C(6) TO C(8,-2,1,0,1,1) 
U(IJ) .0, 0.04000 = C(6) TO C(8,4,2,0,0,-1) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(7) TO C(7,-2,1,0,1,1) 
U(IJ) .0, 0.04000 = C(7) TO C(8) 
U(IJ) .0, 0.04000 = C(8) TO C(8,-2,1,0,1,1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,y+1/2,z+1/2
-x,-y+1/2,-z+1/2
x+1/2,y,z+1/2
-x+1/2,-y,-z+1/2
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y+1/4,z+1/4
x,-y+1/4,-z+1/4
-x,y+3/4,z+3/4
x,-y+3/4,-z+3/4
-x+1/2,y+1/4,z+3/4
x+1/2,-y+1/4,-z+3/4
-x+1/2,y+3/4,z+1/4
x+1/2,-y+3/4,-z+1/4
x+1/4,-y,z+1/4
-x+1/4,y,-z+1/4
x+1/4,-y+1/2,z+3/4
-x+1/4,y+1/2,-z+3/4
x+3/4,-y,z+3/4
-x+3/4,y,-z+3/4
x+3/4,-y+1/2,z+1/4
-x+3/4,y+1/2,-z+1/4
-x+1/4,-y+3/4,z+1/2
x+1/4,y+3/4,-z+1/2
-x+1/4,-y+5/4,z+1
x+1/4,y+5/4,-z+1
-x+3/4,-y+3/4,z+1
x+3/4,y+3/4,-z+1
-x+3/4,-y+5/4,z+1/2
x+3/4,y+5/4,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Sc1 Sc 0.3750 0.3750 0.63579(4) 0.0101 1.0000 Uani S T
O1 O 0.2453(5) 0.3342(2) 0.59247(12) 0.0419 1.0000 Uani . U
O2 O 0.0086(4) 0.3331(2) 0.57042(11) 0.0306 1.0000 Uani . U
O3 O 0.2448(5) 0.45834(17) 0.63548(14) 0.0394 1.0000 Uani . U
C1 C 0.1476(6) 0.3201(3) 0.56726(16) 0.0259 1.0000 Uani . U
C2 C 0.2009(6) 0.2839(3) 0.53229(17) 0.0306 1.0000 Uani . U
C3 C 0.0975(7) 0.2644(4) 0.50463(19) 0.0490 1.0000 Uani . U
C4 C 0.1466(7) 0.2306(4) 0.47237(19) 0.0503 1.0000 Uani . U
C5 C 0.1250 0.4855(3) 0.6250 0.0290 1.0000 Uani S TU
C6 C 0.1250 0.5586(3) 0.6250 0.0294 1.0000 Uani S TU
C7 C 0.258(3) 0.5939(13) 0.6179(7) 0.0340 0.5000 Uani . U
C8 C 0.258(3) 0.6607(13) 0.6173(7) 0.0344 0.5000 Uani . U
H31 H -0.0082 0.2743 0.5077 0.0575 1.0000 Uiso . .
H41 H 0.0752 0.2171 0.4533 0.0604 1.0000 Uiso . .
H71 H 0.3507 0.5712 0.6137 0.0412 0.5000 Uiso . .
H81 H 0.3488 0.6841 0.6115 0.0418 0.5000 Uiso . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sc 0.2519 0.3716 9.1890 9.0213 7.3679 0.5729 1.6409 136.1080 1.4680 51.3531
1.3329 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 18_556 Sc1 O2 16_556 88.2(2) yes
O2 18_556 Sc1 O3 29_554 88.01(17) yes
O2 16_556 Sc1 O3 29_554 92.42(18) yes
O2 18_556 Sc1 O1 29_554 179.49(18) yes
O2 16_556 Sc1 O1 29_554 92.25(17) yes
O3 29_554 Sc1 O1 29_554 92.00(19) yes
O2 18_556 Sc1 O1 . 92.25(17) yes
O2 16_556 Sc1 O1 . 179.49(18) yes
O3 29_554 Sc1 O1 . 87.57(18) yes
O1 29_554 Sc1 O1 . 87.2(3) yes
O2 18_556 Sc1 O3 . 92.42(18) yes
O2 16_556 Sc1 O3 . 88.01(17) yes
O3 29_554 Sc1 O3 . 179.4(3) yes
O1 29_554 Sc1 O3 . 87.57(19) yes
O1 . Sc1 O3 . 92.00(19) yes
Sc1 . O1 C1 . 167.2(4) yes
Sc1 16_456 O2 C1 . 134.0(4) yes
Sc1 . O3 C5 . 147.6(4) yes
O2 . C1 O1 . 123.7(5) yes
O2 . C1 C2 . 118.9(5) yes
O1 . C1 C2 . 117.4(5) yes
C1 . C2 C4 8_556 120.4(5) yes
C1 . C2 C3 . 119.9(5) yes
C4 8_556 C2 C3 . 119.7(5) yes
C2 . C3 C4 . 119.9(5) yes
C2 . C3 H31 . 120.1 no
C4 . C3 H31 . 120.0 no
C3 . C4 C2 8_556 120.4(5) yes
C3 . C4 H41 . 119.8 no
C2 8_556 C4 H41 . 119.7 no
O3 . C5 O3 18_556 126.2(7) yes
O3 . C5 C6 . 116.9(3) yes
O3 18_556 C5 C6 . 116.9(3) yes
C5 . C6 C7 18_556 121.5(10) yes
C5 . C6 C8 27_554 117.9(11) yes
C7 18_556 C6 C8 27_554 21.5(16) yes
C5 . C6 C8 10_566 117.9(11) yes
C7 18_556 C6 C8 10_566 116.2(9) yes
C8 27_554 C6 C8 10_566 124(2) yes
C5 . C6 C7 . 121.5(10) yes
C7 18_556 C6 C7 . 117(2) yes
C8 27_554 C6 C7 . 116.2(9) yes
C8 10_566 C6 C7 . 21.5(16) yes
H81 10_566 C7 C6 . 101.3 no
H81 10_566 C7 C7 10_566 104.1 no
C6 . C7 C7 10_566 115.4(15) yes
H81 10_566 C7 C8 . 119.0 no
C6 . C7 C8 . 122(2) yes
C7 10_566 C7 C8 . 21.5(16) yes
H81 10_566 C7 H71 . 44.9 no
C6 . C7 H71 . 118.8 no
C7 10_566 C7 H71 . 121.2 no
C8 . C7 H71 . 119.3 no
H71 10_566 C8 C8 10_566 96.9 no
H71 10_566 C8 C7 . 109.4 no
C8 10_566 C8 C7 . 18.7(17) yes
H71 10_566 C8 C6 10_566 110.9 no
C8 10_566 C8 C6 10_566 112.0(12) yes
C7 . C8 C6 10_566 118(2) yes
H71 10_566 C8 H81 . 48.8 no
C8 10_566 C8 H81 . 123.5 no
C7 . C8 H81 . 121.1 no
C6 10_566 C8 H81 . 121.4 no
C8 10_566 H71 C7 . 27.8 no
C7 10_566 H81 C8 . 23.9 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sc1 O2 18_556 2.098(4) yes
Sc1 O2 16_556 2.098(4) yes
Sc1 O3 29_554 2.074(4) yes
Sc1 O1 29_554 2.057(4) yes
Sc1 O1 . 2.057(4) yes
Sc1 O3 . 2.074(4) yes
O1 C1 . 1.254(7) yes
O2 C1 . 1.254(7) yes
O3 C5 . 1.247(5) yes
C1 C2 . 1.493(7) yes
C2 C4 8_556 1.381(9) yes
C2 C3 . 1.376(8) yes
C3 C4 . 1.382(8) yes
C3 H31 . 0.955 no
C4 H41 . 0.948 no
C5 C6 . 1.519(9) yes
C6 C7 18_556 1.40(2) yes
C6 C8 27_554 1.36(2) yes
C6 C8 10_566 1.36(2) yes
C6 C7 . 1.40(2) yes
C7 H81 10_566 1.214 no
C7 C7 10_566 1.38(6) yes
C7 C8 . 1.389(12) yes
C7 H71 . 0.951 no
C8 H71 10_566 1.106 no
C8 C8 10_566 1.58(5) yes
C8 H81 . 0.950 no
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
0 22 2 x
1 11 33 x
0 10 34 x
1 13 31 x
2 22 8 x
1 9 35 x
0 22 10 x
1 13 29 x
0 12 32 x
0 14 30 x
1 11 31 x
0 22 6 x
