#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/20/4502022.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_4502022
loop_
_publ_author_name
'Davies, Robert P.'
'Less, Rob'
'Lickiss, Paul D.'
'Robertson, Karen'
'White, Andrew J. P.'
_publ_section_title
;
 Structural Diversity in Metal−Organic Frameworks Built from Rigid
 Tetrahedral [Si(p-C6H4CO2)4]4−Struts
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4571
_journal_paper_doi               10.1021/cg1008768
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C14 H10 Mn O5 Si0.5, 1.25(C4 H9 N O)'
_chemical_formula_sum            'C19 H21.25 Mn N1.25 O6.25 Si0.5'
_chemical_formula_weight         436.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.070(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.0355(18)
_cell_length_b                   22.908(4)
_cell_length_c                   13.882(4)
_cell_measurement_reflns_used    26119
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.7664
_cell_measurement_theta_min      3.1862
_cell_volume                     4139.5(15)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54248
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            50287
_diffrn_reflns_theta_full        70.98
_diffrn_reflns_theta_max         70.98
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    5.783
_exptl_absorpt_correction_T_max  1.09205
_exptl_absorpt_correction_T_min  0.87399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) 
(compiled May 11 2006,17:41:17) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
 SQUEEZE suggests 494 e/cell = 61.8 e/asu.
 The solvent used was dma = C4H9NO = 48e
 1.25dma = 60e, so this was used as the solvent present.
;
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3988
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0587P)²+0.5783P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                3387
_reflns_number_total             3988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1008768_si_001.cif
_cod_data_source_block           IMP-8Mn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      I2/a
_cod_original_formula_sum        'C19 H21.25 Mn N1.25 O6.25 Si0.50'
_cod_database_code               4502022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mn1 Mn 0.2500 0.185198(15) 0.5000 0.03014(11) Uani 1 2 d S
Mn2 Mn 0.2500 0.2500 0.2500 0.03183(11) Uani 1 2 d S
O1 O 0.09908(12) 0.26003(7) 0.30096(11) 0.0531(4) Uani 1 1 d D
H1A H 0.0951(19) 0.2556(10) 0.3651(3) 0.058(7) Uiso 1 1 d D
H1B H 0.0382(16) 0.2549(17) 0.268(3) 0.141(17) Uiso 1 1 d D
Si Si 0.7500 0.45308(2) 0.5000 0.02842(14) Uani 1 2 d S
C1 C 0.63450(13) 0.40472(7) 0.48724(11) 0.0320(3) Uani 1 1 d .
C2 C 0.63126(15) 0.35266(8) 0.53941(13) 0.0419(4) Uani 1 1 d .
H2A H 0.6863 0.3434 0.5844 0.050 Uiso 1 1 calc R
C3 C 0.54961(15) 0.31423(8) 0.52696(13) 0.0408(4) Uani 1 1 d .
H3A H 0.5495 0.2790 0.5631 0.049 Uiso 1 1 calc R
C4 C 0.46810(13) 0.32675(7) 0.46218(12) 0.0315(3) Uani 1 1 d .
C5 C 0.46917(15) 0.37857(8) 0.41113(15) 0.0440(4) Uani 1 1 d .
H5A H 0.4134 0.3880 0.3670 0.053 Uiso 1 1 calc R
C6 C 0.55098(15) 0.41674(8) 0.42395(14) 0.0441(4) Uani 1 1 d .
H6A H 0.5500 0.4522 0.3884 0.053 Uiso 1 1 calc R
C7 C 0.38071(13) 0.28483(7) 0.44528(12) 0.0325(4) Uani 1 1 d .
O8 O 0.37521(10) 0.24285(5) 0.50439(9) 0.0364(3) Uani 1 1 d .
O9 O 0.31825(10) 0.29333(5) 0.37499(9) 0.0378(3) Uani 1 1 d .
C11 C 0.74331(13) 0.50167(7) 0.60834(12) 0.0323(4) Uani 1 1 d .
C12 C 0.80636(14) 0.55107(7) 0.61633(13) 0.0356(4) Uani 1 1 d .
H12A H 0.8537 0.5585 0.5681 0.043 Uiso 1 1 calc R
C13 C 0.80106(14) 0.58925(7) 0.69298(13) 0.0362(4) Uani 1 1 d .
H13A H 0.8444 0.6226 0.6970 0.043 Uiso 1 1 calc R
C14 C 0.73225(14) 0.57888(7) 0.76418(12) 0.0350(4) Uani 1 1 d .
C15 C 0.67015(15) 0.52946(8) 0.75895(13) 0.0394(4) Uani 1 1 d .
H15A H 0.6242 0.5217 0.8082 0.047 Uiso 1 1 calc R
C16 C 0.67573(15) 0.49137(7) 0.68109(13) 0.0378(4) Uani 1 1 d .
H16A H 0.6328 0.4578 0.6775 0.045 Uiso 1 1 calc R
C17 C 0.72365(15) 0.62126(7) 0.84515(13) 0.0374(4) Uani 1 1 d .
O18 O 0.77151(11) 0.67004(5) 0.84172(9) 0.0403(3) Uani 1 1 d .
O19 O 0.67406(12) 0.60899(6) 0.91693(9) 0.0495(3) Uani 1 1 d .
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'
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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 '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
O8 Mn1 O8 101.97(7) . 2_556
O8 Mn1 O18 89.32(5) . 3_444
O8 Mn1 O18 101.87(5) 2_556 3_444
O8 Mn1 O18 101.87(5) . 4_546
O8 Mn1 O18 89.32(5) 2_556 4_546
O18 Mn1 O18 162.29(6) 3_444 4_546
O8 Mn1 O19 144.09(5) . 3_444
O8 Mn1 O19 98.67(5) 2_556 3_444
O18 Mn1 O19 57.64(5) 3_444 3_444
O18 Mn1 O19 107.48(5) 4_546 3_444
O8 Mn1 O19 98.67(5) . 4_546
O8 Mn1 O19 144.09(5) 2_556 4_546
O18 Mn1 O19 107.48(5) 3_444 4_546
O18 Mn1 O19 57.64(5) 4_546 4_546
O19 Mn1 O19 80.54(8) 3_444 4_546
O1 Mn2 O1 180.0 7 .
O1 Mn2 O9 91.81(6) 7 7
O1 Mn2 O9 88.19(6) . 7
O1 Mn2 O9 88.19(6) 7 .
O1 Mn2 O9 91.81(6) . .
O9 Mn2 O9 180.00(5) 7 .
O1 Mn2 O18 90.62(6) 7 3_444
O1 Mn2 O18 89.38(6) . 3_444
O9 Mn2 O18 96.60(5) 7 3_444
O9 Mn2 O18 83.40(5) . 3_444
O1 Mn2 O18 89.38(6) 7 5_666
O1 Mn2 O18 90.62(6) . 5_666
O9 Mn2 O18 83.40(5) 7 5_666
O9 Mn2 O18 96.60(5) . 5_666
O18 Mn2 O18 180.00(6) 3_444 5_666
C1 Si C1 107.35(10) . 2_656
C1 Si C11 110.82(7) . .
C1 Si C11 110.31(7) 2_656 .
C1 Si C11 110.31(7) . 2_656
C1 Si C11 110.82(7) 2_656 2_656
C11 Si C11 107.25(10) . 2_656
C6 C1 C2 116.91(16) . .
C6 C1 Si 122.83(13) . .
C2 C1 Si 120.20(13) . .
C3 C2 C1 121.49(16) . .
C2 C3 C4 120.47(16) . .
C5 C4 C3 118.83(16) . .
C5 C4 C7 119.89(16) . .
C3 C4 C7 121.27(15) . .
C4 C5 C6 120.37(17) . .
C5 C6 C1 121.92(17) . .
O9 C7 O8 124.41(16) . .
O9 C7 C4 118.64(15) . .
O8 C7 C4 116.95(15) . .
C7 O8 Mn1 121.95(11) . .
C7 O9 Mn2 141.33(11) . .
C16 C11 C12 118.04(15) . .
C16 C11 Si 122.54(13) . .
C12 C11 Si 119.39(13) . .
C13 C12 C11 121.30(16) . .
C12 C13 C14 120.00(16) . .
C13 C14 C15 119.84(16) . .
C13 C14 C17 120.08(16) . .
C15 C14 C17 120.07(16) . .
C14 C15 C16 119.70(17) . .
C15 C16 C11 121.10(16) . .
O19 C17 O18 119.97(16) . .
O19 C17 C14 121.14(16) . .
O18 C17 C14 118.83(16) . .
O19 C17 Mn1 61.29(9) . 3
O18 C17 Mn1 59.89(9) . 3
C14 C17 Mn1 166.64(13) . 3
C17 O18 Mn2 133.44(12) . 3
C17 O18 Mn1 90.68(10) . 3
Mn2 O18 Mn1 114.16(5) 3 3
C17 O19 Mn1 90.12(11) . 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O8 2.0980(12) .
Mn1 O8 2.0980(12) 2_556
Mn1 O18 2.2567(14) 3_444
Mn1 O18 2.2567(14) 4_546
Mn1 O19 2.2879(14) 3_444
Mn1 O19 2.2879(14) 4_546
Mn2 O1 2.1384(15) 7
Mn2 O1 2.1384(15) .
Mn2 O9 2.1499(12) 7
Mn2 O9 2.1499(12) .
Mn2 O18 2.2399(12) 3_444
Mn2 O18 2.2399(12) 5_666
Si C1 1.8700(17) .
Si C1 1.8700(17) 2_656
Si C11 1.8768(17) .
Si C11 1.8768(17) 2_656
C1 C6 1.389(3) .
C1 C2 1.397(2) .
C2 C3 1.385(3) .
C3 C4 1.385(3) .
C4 C5 1.383(2) .
C4 C7 1.499(2) .
C5 C6 1.383(3) .
C7 O9 1.252(2) .
C7 O8 1.269(2) .
C11 C16 1.395(3) .
C11 C12 1.400(2) .
C12 C13 1.382(2) .
C13 C14 1.390(3) .
C14 C15 1.391(3) .
C14 C17 1.494(2) .
C15 C16 1.394(2) .
C17 O19 1.248(2) .
C17 O18 1.282(2) .
C17 Mn1 2.6086(18) 3
O18 Mn2 2.2399(12) 3
O18 Mn1 2.2567(14) 3
O19 Mn1 2.2879(14) 3
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.037 0.449 -0.006 1788 494 ' '
