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#$Date: 2016-03-22 12:22:20 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178947 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/76/4117628.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_4117628
loop_
_publ_author_name
'Ana E. Platero-Prats'
'Víctor A. de la Peña-O'Shea'
'Davide M. Proserpio'
'Natalia Snejko'
'Enrique Gutiérrez-Puebla'
'Ángeles Monge'
_publ_contact_author
;
        Enrique Gutiérrez Puebla
        Department of New Architectures in Materials Chemistry
        Institute of Materials Science of Madrid-CSIC. Spain
;
_publ_contact_author_email       egutierrez@icmm.csic.es
_publ_contact_author_fax         +34-913720623
_publ_contact_author_phone       +34-913349024
_publ_section_title
;
 Insight into the SBU Condensation in Mg Coordination and Supramolecular
 Frameworks: A Combined Experimental and Theoretical Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4762
_journal_page_last               4771
_journal_paper_doi               10.1021/ja210564a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C46 H26 F12 Mg N2 O8'
_chemical_formula_weight         987.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 90.2150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   45.3030(8)
_cell_length_b                   10.6226(2)
_cell_length_c                   8.8701(2)
_cell_measurement_reflns_used    5805
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      58.95
_cell_measurement_theta_min      3.90
_cell_volume                     4268.58(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14912
_diffrn_reflns_theta_full        59.52
_diffrn_reflns_theta_max         59.52
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.6857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0487P)²+2.9961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                2665
_reflns_number_total             3070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210564a_si_001_3.cif
_cod_data_source_block           AEPF15
_cod_database_code               4117628
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
C1 C 0.95979(4) 0.41697(18) 0.9566(2) 0.0453(5) Uani 1 1 d .
C2 C 0.92901(4) 0.37382(18) 0.9162(2) 0.0428(5) Uani 1 1 d .
C3 C 0.91674(4) 0.40154(19) 0.7774(2) 0.0496(5) Uani 1 1 d .
H3 H 0.9270 0.4525 0.7105 0.059 Uiso 1 1 calc R
C4 C 0.91270(4) 0.30275(19) 1.0161(2) 0.0481(5) Uani 1 1 d .
H4 H 0.9202 0.2861 1.1118 0.058 Uiso 1 1 calc R
C5 C 0.88534(4) 0.25608(19) 0.9759(2) 0.0479(5) Uani 1 1 d .
H5 H 0.8747 0.2084 1.0448 0.057 Uiso 1 1 calc R
C6 C 0.88934(4) 0.35472(19) 0.7359(2) 0.0491(5) Uani 1 1 d .
H6 H 0.8816 0.3741 0.6415 0.059 Uiso 1 1 calc R
C7 C 0.87343(4) 0.27931(17) 0.8336(2) 0.0413(4) Uani 1 1 d .
C8 C 0.84480(4) 0.20908(18) 0.7900(2) 0.0412(4) Uani 1 1 d .
C9 C 0.85442(4) 0.07079(19) 0.7657(2) 0.0455(5) Uani 1 1 d .
C10 C 0.83099(4) 0.2571(2) 0.6418(2) 0.0517(5) Uani 1 1 d .
C11 C 0.82098(4) 0.22092(18) 0.9136(2) 0.0430(5) Uani 1 1 d .
C12 C 0.81940(5) 0.3309(2) 0.9966(3) 0.0589(6) Uani 1 1 d .
H12 H 0.8314 0.3987 0.9710 0.071 Uiso 1 1 calc R
C13 C 0.80085(4) 0.12595(19) 0.9460(2) 0.0464(5) Uani 1 1 d .
H13 H 0.8000 0.0548 0.8850 0.056 Uiso 1 1 calc R
C14 C 0.78218(4) 0.13601(19) 1.0672(2) 0.0487(5) Uani 1 1 d .
H14 H 0.7692 0.0707 1.0887 0.058 Uiso 1 1 calc R
C15 C 0.80034(5) 0.3416(2) 1.1165(3) 0.0615(6) Uani 1 1 d .
H15 H 0.7995 0.4166 1.1704 0.074 Uiso 1 1 calc R
C16 C 0.78247(4) 0.24207(19) 1.1576(2) 0.0476(5) Uani 1 1 d .
C17 C 0.76620(4) 0.2480(2) 1.3007(2) 0.0508(5) Uani 1 1 d .
C18 C 1.01270(6) 0.1230(2) 1.2013(3) 0.0743(7) Uani 1 1 d .
C19 C 1.04672(7) 0.2363(3) 1.0690(4) 0.0974(10) Uani 1 1 d .
H19 H 1.0541 0.3136 1.0372 0.117 Uiso 1 1 calc R
C20 C 1.06092(10) 0.1285(5) 1.0227(5) 0.1448(18) Uani 1 1 d .
H20 H 1.0777 0.1336 0.9631 0.174 Uiso 1 1 calc R
C21 C 1.05028(11) 0.0156(5) 1.0646(6) 0.1520(19) Uani 1 1 d .
H21 H 1.0595 -0.0577 1.0323 0.182 Uiso 1 1 calc R
C22 C 1.02541(9) 0.0085(3) 1.1563(5) 0.1139(12) Uani 1 1 d .
C23 C 1.01181(12) -0.1064(3) 1.2064(7) 0.161(2) Uani 1 1 d .
H23 H 1.0199 -0.1829 1.1766 0.193 Uiso 1 1 calc R
F1 F 0.86061(3) 0.01435(11) 0.89533(13) 0.0581(3) Uani 1 1 d .
F2 F 0.83416(3) 0.00004(11) 0.69679(14) 0.0624(3) Uani 1 1 d .
F3 F 0.87869(3) 0.06287(11) 0.68155(13) 0.0586(3) Uani 1 1 d .
F4 F 0.80494(3) 0.20315(14) 0.61416(15) 0.0715(4) Uani 1 1 d .
F5 F 0.84760(3) 0.23656(13) 0.52072(13) 0.0643(4) Uani 1 1 d .
F6 F 0.82625(3) 0.38073(12) 0.64893(16) 0.0693(4) Uani 1 1 d .
Mg1 Mg 1.0000 0.40615(9) 1.2500 0.0430(2) Uani 1 2 d S
N1 N 1.02323(4) 0.23575(18) 1.1560(2) 0.0661(5) Uani 1 1 d .
O1 O 0.96899(3) 0.38904(17) 1.08268(17) 0.0692(5) Uani 1 1 d .
O2 O 0.97353(3) 0.47509(16) 0.85770(19) 0.0706(5) Uani 1 1 d .
O3 O 0.75439(4) 0.14486(14) 1.34618(19) 0.0683(5) Uani 1 1 d .
H3A H 0.7467 0.1562 1.4287 0.102 Uiso 1 1 calc R
O4 O 0.76530(4) 0.34793(14) 1.37496(18) 0.0654(4) 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'
F F 0.0727 0.0534 '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'
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
O1 C1 O2 126.42(19) . .
O1 C1 C2 116.92(18) . .
O2 C1 C2 116.64(18) . .
C4 C2 C3 118.31(18) . .
C4 C2 C1 120.65(17) . .
C3 C2 C1 121.02(17) . .
C2 C3 C6 121.18(18) . .
C2 C3 H3 119.4 . .
C6 C3 H3 119.4 . .
C5 C4 C2 120.83(18) . .
C5 C4 H4 119.6 . .
C2 C4 H4 119.6 . .
C4 C5 C7 121.00(18) . .
C4 C5 H5 119.5 . .
C7 C5 H5 119.5 . .
C7 C6 C3 120.60(18) . .
C7 C6 H6 119.7 . .
C3 C6 H6 119.7 . .
C6 C7 C5 117.98(17) . .
C6 C7 C8 124.16(17) . .
C5 C7 C8 117.60(16) . .
C10 C8 C7 113.04(16) . .
C10 C8 C11 107.20(15) . .
C7 C8 C11 111.79(15) . .
C10 C8 C9 108.01(16) . .
C7 C8 C9 104.88(15) . .
C11 C8 C9 111.94(15) . .
F1 C9 F2 106.61(16) . .
F1 C9 F3 106.55(16) . .
F2 C9 F3 105.98(15) . .
F1 C9 C8 111.54(15) . .
F2 C9 C8 113.91(16) . .
F3 C9 C8 111.77(15) . .
F5 C10 F6 106.96(17) . .
F5 C10 F4 106.44(17) . .
F6 C10 F4 106.83(17) . .
F5 C10 C8 113.91(17) . .
F6 C10 C8 110.56(17) . .
F4 C10 C8 111.75(17) . .
C12 C11 C13 117.87(18) . .
C12 C11 C8 118.94(17) . .
C13 C11 C8 123.19(17) . .
C15 C12 C11 120.98(19) . .
C15 C12 H12 119.5 . .
C11 C12 H12 119.5 . .
C14 C13 C11 120.74(18) . .
C14 C13 H13 119.6 . .
C11 C13 H13 119.6 . .
C13 C14 C16 120.81(18) . .
C13 C14 H14 119.6 . .
C16 C14 H14 119.6 . .
C12 C15 C16 120.7(2) . .
C12 C15 H15 119.7 . .
C16 C15 H15 119.7 . .
C15 C16 C14 118.37(19) . .
C15 C16 C17 119.37(19) . .
C14 C16 C17 122.10(18) . .
O4 C17 O3 122.99(19) . .
O4 C17 C16 120.56(19) . .
O3 C17 C16 116.38(19) . .
N1 C18 C22 122.5(3) . .
N1 C18 C18 117.52(13) . 2_757
C22 C18 C18 120.0(2) . 2_757
N1 C19 C20 123.4(3) . .
N1 C19 H19 118.3 . .
C20 C19 H19 118.3 . .
C21 C20 C19 119.4(4) . .
C21 C20 H20 120.3 . .
C19 C20 H20 120.3 . .
C20 C21 C22 120.0(3) . .
C20 C21 H21 120.0 . .
C22 C21 H21 120.0 . .
C21 C22 C18 116.9(3) . .
C21 C22 C23 125.0(4) . .
C18 C22 C23 118.0(4) . .
C23 C23 C22 121.9(2) 2_757 .
C23 C23 H23 119.0 2_757 .
C22 C23 H23 119.0 . .
O2 Mg1 O2 101.20(11) 6_566 5_767
O2 Mg1 O1 89.50(7) 6_566 .
O2 Mg1 O1 96.97(6) 5_767 .
O2 Mg1 O1 96.97(6) 6_566 2_757
O2 Mg1 O1 89.50(7) 5_767 2_757
O1 Mg1 O1 169.82(11) . 2_757
O2 Mg1 N1 92.78(7) 6_566 2_757
O2 Mg1 N1 166.02(8) 5_767 2_757
O1 Mg1 N1 82.93(7) . 2_757
O1 Mg1 N1 88.89(8) 2_757 2_757
O2 Mg1 N1 166.02(8) 6_566 .
O2 Mg1 N1 92.78(7) 5_767 .
O1 Mg1 N1 88.89(8) . .
O1 Mg1 N1 82.93(7) 2_757 .
N1 Mg1 N1 73.24(11) 2_757 .
C19 N1 C18 117.8(2) . .
C19 N1 Mg1 126.31(19) . .
C18 N1 Mg1 115.82(15) . .
C1 O1 Mg1 150.22(14) . .
C1 O2 Mg1 163.73(15) . 5_767
C17 O3 H3A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.229(2) .
C1 O2 1.242(2) .
C1 C2 1.509(3) .
C2 C4 1.381(3) .
C2 C3 1.381(3) .
C3 C6 1.386(3) .
C3 H3 0.9300 .
C4 C5 1.381(3) .
C4 H4 0.9300 .
C5 C7 1.393(3) .
C5 H5 0.9300 .
C6 C7 1.385(3) .
C6 H6 0.9300 .
C7 C8 1.544(3) .
C8 C10 1.541(3) .
C8 C11 1.546(3) .
C8 C9 1.548(3) .
C9 F1 1.326(2) .
C9 F2 1.333(2) .
C9 F3 1.334(2) .
C10 F5 1.332(2) .
C10 F6 1.332(2) .
C10 F4 1.334(2) .
C11 C12 1.383(3) .
C11 C13 1.391(3) .
C12 C15 1.377(3) .
C12 H12 0.9300 .
C13 C14 1.375(3) .
C13 H13 0.9300 .
C14 C16 1.383(3) .
C14 H14 0.9300 .
C15 C16 1.381(3) .
C15 H15 0.9300 .
C16 C17 1.472(3) .
C17 O4 1.250(3) .
C17 O3 1.285(2) .
C18 N1 1.351(3) .
C18 C22 1.404(4) .
C18 C18 1.441(5) 2_757
C19 N1 1.317(3) .
C19 C20 1.378(5) .
C19 H19 0.9300 .
C20 C21 1.344(6) .
C20 H20 0.9300 .
C21 C22 1.394(6) .
C21 H21 0.9300 .
C22 C23 1.438(5) .
C23 C23 1.323(9) 2_757
C23 H23 0.9300 .
Mg1 O2 1.9876(16) 6_566
Mg1 O2 1.9876(16) 5_767
Mg1 O1 2.0478(14) .
Mg1 O1 2.0478(15) 2_757
Mg1 N1 2.255(2) 2_757
Mg1 N1 2.255(2) .
O2 Mg1 1.9876(16) 5_767
O3 H3A 0.8200 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O4 0.82 1.83 2.634(2) 167.4 7_658
