#------------------------------------------------------------------------------
#$Date: 2019-02-15 01:50:09 +0200 (Fri, 15 Feb 2019) $
#$Revision: 213647 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/23/7232361.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_7232361
loop_
_publ_author_name
'Henkelis, Susan Elizabeth'
'Vornholt, Simon Maximilian'
'Cordes, David Bradford'
'Slawin, Alexandra'
'Wheatley, Paul Stewart S.'
'Morris, Russell'
_publ_section_title
;
 A single crystal study of CPO-27 and UTSA-74 for nitric oxide storage and
 release
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE00098D
_journal_year                    2019
_chemical_formula_moiety         'C8 H6 Mg2 O8'
_chemical_formula_sum            'C8 H6 Mg2 O8'
_chemical_formula_weight         278.75
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-07-05
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2018-08-23 deposited with the CCDC.
2019-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.9434(9)
_cell_length_b                   25.9434(9)
_cell_length_c                   6.8189(2)
_cell_measurement_reflns_used    3392
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      67.7090
_cell_measurement_theta_min      3.3980
_cell_volume                     3974.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku XtaLAB P100'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14270
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         3.407
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43i (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_description       needle
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1617
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0624
_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)+(0.0918P)²+20.9238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1285
_reflns_number_total             1617
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00098d2.cif
_cod_data_source_block           CPO-27-Mg
_cod_original_cell_volume        3974.6(3)
_cod_database_code               7232361
_shelx_shelxl_version_number     2018/3
_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   0.931
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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'
'-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'
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
Mg01 Mg 0.36784(5) 0.05165(5) 0.51949(15) 0.0214(4) Uani 1 1 d .
O002 O 0.34272(11) 0.03695(10) 0.9787(3) 0.0218(6) Uani 1 1 d .
O003 O 0.35687(11) 0.27341(11) 0.9958(3) 0.0224(6) Uani 1 1 d .
O004 O 0.36582(12) 0.10277(11) 0.7412(3) 0.0267(6) Uani 1 1 d .
C006 C 0.34933(15) 0.08587(16) 0.9140(5) 0.0223(8) Uani 1 1 d .
C007 C 0.34438(16) 0.22196(16) 1.0829(5) 0.0237(8) Uani 1 1 d .
C008 C 0.33900(16) 0.12495(17) 1.0494(5) 0.0242(8) Uani 1 1 d .
C009 C 0.34947(16) 0.17937(17) 0.9743(5) 0.0251(8) Uani 1 1 d .
H009 H 0.360800 0.187866 0.840545 0.030 Uiso 1 1 calc R
O1 O 0.44189(13) 0.12139(13) 0.3863(4) 0.0382(7) Uani 1 1 d D
H1A H 0.4743(10) 0.1581(10) 0.4496(13) 0.057 Uiso 1 1 d DGR
H1B H 0.4532(10) 0.1258(9) 0.244(2) 0.057 Uiso 1 1 d DGR
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'
Mg Mg 0.1719 0.1771 '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
Mg01 Mg01 Mg01 109.15(4) 6 8_544
O002 Mg01 Mg01 73.05(7) 8_544 8_544
O002 Mg01 Mg01 42.31(7) 8_544 6
O002 Mg01 Mg01 44.34(7) 6_554 8_544
O002 Mg01 Mg01 91.39(8) 6_554 6
O002 Mg01 O002 80.60(4) 6_554 8_544
O002 Mg01 O1 93.23(12) 6_554 .
O003 Mg01 Mg01 41.27(7) 13_556 8_544
O003 Mg01 Mg01 124.95(9) 18_546 8_544
O003 Mg01 Mg01 41.51(8) 18_546 6
O003 Mg01 Mg01 132.91(9) 13_556 6
O003 Mg01 O002 90.83(10) 13_556 8_544
O003 Mg01 O002 81.29(10) 18_546 8_544
O003 Mg01 O002 83.00(10) 13_556 6_554
O003 Mg01 O002 84.44(10) 18_546 6_554
O003 Mg01 O003 166.12(11) 18_546 13_556
O003 Mg01 O1 92.99(11) 13_556 .
O003 Mg01 O1 93.60(12) 18_546 .
O004 Mg01 Mg01 133.23(10) . 8_544
O004 Mg01 Mg01 83.19(7) . 6
O004 Mg01 O002 172.65(11) . 6_554
O004 Mg01 O002 92.05(10) . 8_544
O004 Mg01 O003 97.05(11) . 13_556
O004 Mg01 O003 94.66(11) . 18_546
O004 Mg01 O1 94.10(12) . .
O1 Mg01 Mg01 134.08(11) . 6
O1 Mg01 Mg01 105.73(9) . 8_544
O1 Mg01 O002 172.31(13) . 8_544
Mg01 O002 Mg01 93.34(9) 8_545 6
C006 O002 Mg01 134.5(2) . 6
C006 O002 Mg01 126.3(2) . 8_545
Mg01 O003 Mg01 97.23(11) 17_556 13_556
C007 O003 Mg01 122.8(2) . 17_556
C007 O003 Mg01 123.2(2) . 13_556
C006 O004 Mg01 125.9(2) . .
O002 C006 C008 118.9(3) . .
O004 C006 O002 121.8(3) . .
O004 C006 C008 119.3(3) . .
O003 C007 C008 124.2(3) . 13_557
O003 C007 C009 118.9(3) . .
C009 C007 C008 116.9(3) . 13_557
C007 C008 C006 124.2(3) 13_557 .
C009 C008 C006 116.8(3) . .
C009 C008 C007 118.9(3) . 13_557
C007 C009 C008 124.2(3) . .
C007 C009 H009 117.9 . .
C008 C009 H009 117.9 . .
Mg01 O1 H1A 127.7 . .
Mg01 O1 H1B 127.8 . .
H1A O1 H1B 104.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg01 Mg01 3.0592(13) 8_544
Mg01 Mg01 3.0591(13) 6
Mg01 O002 2.142(3) 8_544
Mg01 O002 2.063(3) 6_554
Mg01 O003 2.044(3) 13_556
Mg01 O003 2.034(3) 18_546
Mg01 O004 2.029(3) .
Mg01 O1 2.077(3) .
O002 C006 1.271(4) .
O003 C007 1.344(4) .
O004 C006 1.256(4) .
C006 C008 1.491(5) .
C007 C008 1.428(5) 13_557
C007 C009 1.390(5) .
C008 C009 1.395(5) .
C009 H009 0.9500 .
O1 H1A 0.999(14) .
O1 H1B 1.000(14) .
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 0.000 0.000 -0.734 701.4 181.8
2 0.333 0.667 -0.082 701.4 181.8
3 0.667 0.333 -0.415 701.4 181.8
