#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:22:20 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178947 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/76/4117626.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_4117626
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            'C29 H24 F6 Mg N2 O8'
_chemical_formula_weight         666.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.8630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2022(2)
_cell_length_b                   7.61350(10)
_cell_length_c                   31.0128(5)
_cell_measurement_reflns_used    5390
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      58.15
_cell_measurement_theta_min      2.89
_cell_volume                     3071.18(8)
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            23890
_diffrn_reflns_theta_full        62.38
_diffrn_reflns_theta_max         62.38
_diffrn_reflns_theta_min         2.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.7807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         4821
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0464
_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)+(0.0603P)²+1.6736P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                3626
_reflns_number_total             4821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210564a_si_001_1.cif
_cod_data_source_block           alphaAEPF14
_cod_database_code               4117626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
C1 C 0.7003(2) 0.8097(4) 0.90059(9) 0.0631(8) Uani 1 1 d .
H1 H 0.7651 0.8069 0.8926 0.076 Uiso 1 1 calc R
C2 C 0.6159(3) 0.8502(5) 0.86865(10) 0.0822(10) Uani 1 1 d .
H2 H 0.6248 0.8761 0.8402 0.099 Uiso 1 1 calc R
C3 C 0.5206(3) 0.8514(5) 0.87940(12) 0.0891(11) Uani 1 1 d .
H3 H 0.4637 0.8772 0.8583 0.107 Uiso 1 1 calc R
C4 C 0.5079(2) 0.8138(4) 0.92215(11) 0.0671(8) Uani 1 1 d .
C5 C 0.5969(2) 0.7787(3) 0.95272(9) 0.0493(6) Uani 1 1 d .
C6 C 0.4106(3) 0.8119(5) 0.93623(15) 0.0903(12) Uani 1 1 d .
H6 H 0.3514 0.8362 0.9161 0.108 Uiso 1 1 calc R
C7 C 0.4026(3) 0.7759(5) 0.97766(15) 0.0898(12) Uani 1 1 d .
H7 H 0.3379 0.7728 0.9857 0.108 Uiso 1 1 calc R
C8 C 0.4909(2) 0.7423(4) 1.00966(11) 0.0653(8) Uani 1 1 d .
C9 C 0.58862(19) 0.7455(3) 0.99756(9) 0.0484(6) Uani 1 1 d .
C10 C 0.4863(3) 0.7077(5) 1.05363(13) 0.0817(10) Uani 1 1 d .
H10 H 0.4231 0.7035 1.0630 0.098 Uiso 1 1 calc R
C11 C 0.5736(3) 0.6808(5) 1.08214(12) 0.0809(10) Uani 1 1 d .
H11 H 0.5711 0.6573 1.1114 0.097 Uiso 1 1 calc R
C12 C 0.6681(2) 0.6883(4) 1.06776(10) 0.0645(8) Uani 1 1 d .
H12 H 0.7278 0.6704 1.0880 0.077 Uiso 1 1 calc R
N2 N 0.67631(16) 0.7197(3) 1.02654(7) 0.0485(5) Uani 1 1 d .
C13 C 0.8286(2) 0.1986(3) 0.90721(8) 0.0463(6) Uani 1 1 d .
C14 C 0.8085(2) 0.2972(3) 0.86438(8) 0.0473(6) Uani 1 1 d .
C16 C 0.7188(3) 0.3863(4) 0.85136(9) 0.0682(9) Uani 1 1 d .
H16 H 0.6683 0.3840 0.8689 0.082 Uiso 1 1 calc R
C15 C 0.8818(2) 0.3008(4) 0.83759(9) 0.0630(8) Uani 1 1 d .
H15 H 0.9429 0.2390 0.8456 0.076 Uiso 1 1 calc R
C18 C 0.8657(3) 0.3945(4) 0.79926(9) 0.0682(8) Uani 1 1 d .
H18 H 0.9162 0.3958 0.7817 0.082 Uiso 1 1 calc R
C17 C 0.7015(3) 0.4799(5) 0.81266(9) 0.0788(10) Uani 1 1 d .
H17 H 0.6395 0.5387 0.8043 0.095 Uiso 1 1 calc R
C19 C 0.7760(3) 0.4866(4) 0.78635(8) 0.0647(8) Uani 1 1 d .
C20 C 0.7669(3) 0.5995(4) 0.74437(9) 0.0860(12) Uani 1 1 d .
C22 C 0.6570(7) 0.6620(9) 0.72946(17) 0.162(4) Uani 1 1 d .
C21 C 0.8403(6) 0.7598(5) 0.75613(14) 0.125(2) Uani 1 1 d .
C23 C 0.7963(3) 0.4922(4) 0.70592(8) 0.0657(9) Uani 1 1 d .
C24 C 0.8436(3) 0.5644(4) 0.67348(9) 0.0784(10) Uani 1 1 d .
H24 H 0.8597 0.6834 0.6744 0.094 Uiso 1 1 calc R
C25 C 0.7712(3) 0.3166(4) 0.70269(9) 0.0631(8) Uani 1 1 d .
H25 H 0.7370 0.2662 0.7235 0.076 Uiso 1 1 calc R
C26 C 0.8670(3) 0.4618(4) 0.63978(9) 0.0655(8) Uani 1 1 d .
H26 H 0.8979 0.5132 0.6181 0.079 Uiso 1 1 calc R
C27 C 0.7955(2) 0.2142(4) 0.66941(8) 0.0571(7) Uani 1 1 d .
H27 H 0.7782 0.0957 0.6681 0.069 Uiso 1 1 calc R
C28 C 0.8455(2) 0.2855(3) 0.63772(8) 0.0463(6) Uani 1 1 d .
C29 C 0.87427(19) 0.1668(3) 0.60296(8) 0.0458(6) Uani 1 1 d .
F1 F 0.9379(3) 0.7132(4) 0.76133(9) 0.1486(14) Uani 1 1 d .
F2 F 0.8244(4) 0.8878(3) 0.72777(8) 0.204(2) Uani 1 1 d .
F3 F 0.8241(3) 0.8286(3) 0.79473(7) 0.1752(16) Uani 1 1 d .
F4 F 0.6487(3) 0.7451(5) 0.68988(7) 0.201(2) Uani 1 1 d .
F5 F 0.5901(3) 0.5336(6) 0.72403(10) 0.1573(18) Uani 1 1 d .
F6 F 0.6261(3) 0.7826(4) 0.75564(8) 0.1945(19) Uani 1 1 d .
H1A H 0.803(2) 0.400(4) 0.9712(9) 0.087(11) Uiso 1 1 d D
H2A H 0.922(2) 0.908(3) 0.9442(10) 0.086(10) Uiso 1 1 d D
H3A H 0.912(3) 0.635(4) 1.0776(10) 0.113(13) Uiso 1 1 d D
H4A H 0.795(3) 1.092(4) 0.9801(8) 0.095(11) Uiso 1 1 d D
H1B H 0.854(3) 0.414(4) 1.0208(8) 0.110(13) Uiso 1 1 d D
H2B H 0.985(2) 0.743(5) 0.9507(13) 0.120(14) Uiso 1 1 d D
H3B H 0.9764(19) 0.797(4) 1.0648(11) 0.094(11) Uiso 1 1 d D
H4B H 0.843(2) 1.081(4) 1.0306(8) 0.099(12) Uiso 1 1 d D
Mg1 Mg 0.82065(6) 0.74788(10) 0.99828(3) 0.0417(2) Uani 1 1 d .
N1 N 0.69276(17) 0.7751(3) 0.94181(7) 0.0483(5) Uani 1 1 d .
O1 O 0.83104(16) 0.4809(2) 0.99398(6) 0.0573(5) Uani 1 1 d D
O2 O 0.92326(15) 0.7933(3) 0.95766(7) 0.0651(6) Uani 1 1 d D
O3 O 0.91321(15) 0.7331(3) 1.05670(6) 0.0586(5) Uani 1 1 d D
O4 O 0.81104(15) 1.0148(2) 1.00533(6) 0.0522(5) Uani 1 1 d D
O5 O 0.76702(15) 0.2221(2) 0.93342(6) 0.0557(5) Uani 1 1 d .
O6 O 0.90595(14) 0.1007(3) 0.91407(6) 0.0591(5) Uani 1 1 d .
O7 O 0.88539(14) 0.2336(2) 0.56671(5) 0.0526(5) Uani 1 1 d .
O8 O 0.88348(17) 0.0085(2) 0.61202(6) 0.0666(6) 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
N1 C1 C2 123.1(3) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C3 C2 C1 119.3(3) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C2 C3 C4 120.0(3) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C3 C4 C5 117.3(3) . .
C3 C4 C6 123.7(3) . .
C5 C4 C6 119.0(3) . .
N1 C5 C4 122.7(3) . .
N1 C5 C9 117.7(2) . .
C4 C5 C9 119.6(3) . .
C7 C6 C4 121.3(3) . .
C7 C6 H6 119.3 . .
C4 C6 H6 119.3 . .
C6 C7 C8 121.3(3) . .
C6 C7 H7 119.3 . .
C8 C7 H7 119.3 . .
C10 C8 C9 117.3(3) . .
C10 C8 C7 123.2(3) . .
C9 C8 C7 119.5(3) . .
N2 C9 C8 122.8(3) . .
N2 C9 C5 118.1(2) . .
C8 C9 C5 119.2(3) . .
C11 C10 C8 119.6(3) . .
C11 C10 H10 120.2 . .
C8 C10 H10 120.2 . .
C10 C11 C12 119.8(3) . .
C10 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
N2 C12 C11 122.8(3) . .
N2 C12 H12 118.6 . .
C11 C12 H12 118.6 . .
C12 N2 C9 117.8(2) . .
C12 N2 Mg1 127.67(19) . .
C9 N2 Mg1 114.51(16) . .
O6 C13 O5 125.0(2) . 1
O6 C13 O5 125.0(2) . .
O5 C13 O5 0.00(14) 1 .
O6 C13 C14 117.5(2) . .
O5 C13 C14 117.6(2) 1 .
O5 C13 C14 117.6(2) . .
C16 C14 C15 118.3(2) . .
C16 C14 C13 121.4(2) . .
C15 C14 C13 120.2(2) . .
C14 C16 C17 121.3(3) . .
C14 C16 H16 119.3 . .
C17 C16 H16 119.3 . .
C18 C15 C14 120.8(3) . .
C18 C15 H15 119.6 . .
C14 C15 H15 119.6 . .
C15 C18 C19 121.0(3) . .
C15 C18 H18 119.5 . .
C19 C18 H18 119.5 . .
C16 C17 C19 120.2(3) . .
C16 C17 H17 119.9 . .
C19 C17 H17 119.9 . .
C18 C19 C17 118.3(3) . .
C18 C19 C20 117.8(3) . .
C17 C19 C20 123.8(3) . .
C22 C20 C19 111.2(4) . .
C22 C20 C23 106.4(3) . .
C19 C20 C23 111.1(2) . .
C22 C20 C21 110.4(4) . .
C19 C20 C21 106.4(3) . .
C23 C20 C21 111.4(3) . .
F5 C22 F6 108.8(7) . .
F5 C22 F4 106.3(6) . .
F6 C22 F4 104.0(4) . .
F5 C22 C20 113.2(5) . .
F6 C22 C20 113.9(6) . .
F4 C22 C20 110.1(6) . .
F2 C21 F1 108.9(6) . .
F2 C21 F3 106.0(3) . .
F1 C21 F3 107.1(5) . .
F2 C21 C20 113.9(5) . .
F1 C21 C20 111.8(4) . .
F3 C21 C20 108.9(5) . .
C25 C23 C24 117.8(3) . .
C25 C23 C20 118.6(3) . .
C24 C23 C20 123.6(3) . .
C26 C24 C23 120.8(3) . .
C26 C24 H24 119.6 . .
C23 C24 H24 119.6 . .
C27 C25 C23 121.4(3) . .
C27 C25 H25 119.3 . .
C23 C25 H25 119.3 . .
C28 C26 C24 121.2(3) . .
C28 C26 H26 119.4 . .
C24 C26 H26 119.4 . .
C25 C27 C28 120.7(3) . .
C25 C27 H27 119.6 . .
C28 C27 H27 119.6 . .
C26 C28 C27 118.1(2) . .
C26 C28 C29 123.1(2) . .
C27 C28 C29 118.8(2) . .
O8 C29 O7 124.8(2) . .
O8 C29 C28 116.7(2) . .
O7 C29 C28 118.5(2) . .
O3 Mg1 O2 101.64(9) . .
O3 Mg1 O1 88.04(8) . .
O2 Mg1 O1 93.99(9) . .
O3 Mg1 O4 89.91(8) . .
O2 Mg1 O4 87.56(8) . .
O1 Mg1 O4 177.65(8) . .
O3 Mg1 N1 168.07(9) . .
O2 Mg1 N1 89.58(9) . .
O1 Mg1 N1 95.26(8) . .
O4 Mg1 N1 86.52(8) . .
O3 Mg1 N2 93.94(9) . .
O2 Mg1 N2 164.01(9) . .
O1 Mg1 N2 90.07(8) . .
O4 Mg1 N2 88.90(8) . .
N1 Mg1 N2 74.64(8) . .
C1 N1 C5 117.5(2) . .
C1 N1 Mg1 127.2(2) . .
C5 N1 Mg1 114.68(17) . .
Mg1 O1 H1A 132(2) . .
Mg1 O1 H1B 118(2) . .
H1A O1 H1B 109(3) . .
Mg1 O2 H2A 117.1(19) . .
Mg1 O2 H2B 139(2) . .
H2A O2 H2B 102(3) . .
Mg1 O3 H3A 124(2) . .
Mg1 O3 H3B 125(2) . .
H3A O3 H3B 109(3) . .
Mg1 O4 H4A 122(2) . .
Mg1 O4 H4B 125(2) . .
H4A O4 H4B 110(3) . .
O5 O5 C13 0(10) 1 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.326(3) .
C1 C2 1.393(5) .
C1 H1 0.9300 .
C2 C3 1.355(5) .
C2 H2 0.9300 .
C3 C4 1.394(5) .
C3 H3 0.9300 .
C4 C5 1.404(4) .
C4 C6 1.426(5) .
C5 N1 1.365(3) .
C5 C9 1.436(4) .
C6 C7 1.335(5) .
C6 H6 0.9300 .
C7 C8 1.418(5) .
C7 H7 0.9300 .
C8 C10 1.401(5) .
C8 C9 1.404(4) .
C9 N2 1.353(3) .
C10 C11 1.343(5) .
C10 H10 0.9300 .
C11 C12 1.397(4) .
C11 H11 0.9300 .
C12 N2 1.323(3) .
C12 H12 0.9300 .
N2 Mg1 2.240(2) .
C13 O6 1.253(3) .
C13 O5 1.257(3) 1
C13 O5 1.257(3) .
C13 C14 1.509(4) .
C14 C16 1.364(4) .
C14 C15 1.380(4) .
C16 C17 1.381(4) .
C16 H16 0.9300 .
C15 C18 1.371(4) .
C15 H15 0.9300 .
C18 C19 1.376(4) .
C18 H18 0.9300 .
C17 C19 1.383(4) .
C17 H17 0.9300 .
C19 C20 1.548(4) .
C20 C22 1.522(8) .
C20 C23 1.549(4) .
C20 C21 1.561(7) .
C22 F5 1.309(9) .
C22 F6 1.335(6) .
C22 F4 1.368(5) .
C21 F2 1.305(5) .
C21 F1 1.320(7) .
C21 F3 1.356(5) .
C23 C25 1.377(4) .
C23 C24 1.385(4) .
C24 C26 1.382(4) .
C24 H24 0.9300 .
C25 C27 1.375(4) .
C25 H25 0.9300 .
C26 C28 1.371(4) .
C26 H26 0.9300 .
C27 C28 1.386(4) .
C27 H27 0.9300 .
C28 C29 1.504(3) .
C29 O8 1.239(3) .
C29 O7 1.265(3) .
Mg1 O3 2.007(2) .
Mg1 O2 2.031(2) .
Mg1 O1 2.0436(19) .
Mg1 O4 2.0498(19) .
Mg1 N1 2.224(2) .
O1 H1A 0.959(18) .
O1 H1B 0.979(19) .
O2 H2A 0.967(18) .
O2 H2B 0.961(19) .
O3 H3A 0.990(19) .
O3 H3B 0.960(19) .
O4 H4A 0.975(18) .
O4 H4B 0.967(19) .
O5 O5 0.000(5) 1
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 O8 0.990(19) 1.62(2) 2.591(3) 167(4) 4_566
O1 H1B O7 0.979(19) 1.80(2) 2.777(2) 172(3) 4_566
O3 H3B O6 0.960(19) 1.762(19) 2.717(3) 173(3) 3_767
O2 H2A O6 0.967(18) 1.732(19) 2.693(3) 171(3) 1_565
O4 H4A O5 0.975(18) 1.738(19) 2.713(2) 177(3) 1_565
O2 H2B O7 0.961(19) 1.88(2) 2.795(3) 159(4) 2_756
O4 H4B O7 0.967(19) 1.83(2) 2.760(3) 161(3) 4_576
O1 H1A O5 0.959(18) 1.803(19) 2.753(3) 170(3) 1
