 
data_FDM-22
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C28 H18 N O4 Zn' 
_chemical_formula_weight          497.80

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 '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'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn'  'Zn'   0.2839   1.4301
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            12
_space_group_name_H-M_alt         'C 2/m'
_space_group_name_Hall            '-C 2y'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'
 
_cell_length_a                    22.03(4)
_cell_length_b                    21.02(4)
_cell_length_c                    15.27(3)
_cell_angle_alpha                 90
_cell_angle_beta                  131.61(3)
_cell_angle_gamma                 90
_cell_volume                      5287(16)
_cell_formula_units_Z             4
_cell_measurement_temperature     258(2)
_cell_measurement_reflns_used     257
_cell_measurement_theta_min       2.32
_cell_measurement_theta_max       19.54
 
_exptl_crystal_description        cuboid
_exptl_crystal_colour             yellow
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     0.625          
_exptl_crystal_F_000              1020
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.32
_exptl_crystal_size_mid           0.21
_exptl_crystal_size_min           0.13
_exptl_absorpt_coefficient_mu     0.480
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'none'
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       258(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'CCD area detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             8490
_diffrn_reflns_av_unetI/netI      0.1942
_diffrn_reflns_av_R_equivalents   0.3005
_diffrn_reflns_limit_h_min        -20
_diffrn_reflns_limit_h_max        21
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          1.649
_diffrn_reflns_theta_max          20.290
_diffrn_reflns_theta_full         20.290
_diffrn_measured_fraction_theta_max   0.959
_diffrn_measured_fraction_theta_full  0.959
_diffrn_reflns_Laue_measured_fraction_max    0.959
_diffrn_reflns_Laue_measured_fraction_full   0.959
_diffrn_reflns_point_group_measured_fraction_max   0.959
_diffrn_reflns_point_group_measured_fraction_full  0.959
_reflns_number_total              2557
_reflns_number_gt                 1686
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

# SQUEEZE RESULTS (Version = 120416)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.008 -0.007 -0.016      3270       947 '1(C5H11NO) '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

In the checkcif report£¬ the three unsolved Alert level A that described as 
The value of Rint is greater than 0.25£¬The value of Rint is greater than 0.12,
and The value of sine(theta_max)/wavelength is less than 0.550, Calculated 
sin(theta_max)/wavelength = 0.4879 were ascribed to poor single crystal quality
and interfering diffraction. We found that the perfect crystals without any 
cracks under optic microscope were finally proved to be twin crystals or crystals
with multi-domains by single-crystal X-ray diffraction, and this problem 
presented in more than 30 crystals we picked out. Analyzed by the cell_now 
program, diffractions from most of these crystals can be divided into more than
3 different domains. We tried several strategies to address the crystals with 
multiple domains. Even though larger crystal was selected, a better data was not 
obtained in more than 10 diffraction collection experiments.

In the SQUEEZE application, the count electrons (947 per unit cell calculated from PLATON) 
correspond to 237 electrons from disordered solvents in each formula.
While it is impossible to determine the exact contents in the voids, we suggest five
DMA molecules per formula. Thus the formula of FDM-22 including the solvents is [Zn2(BPDC)2(BP4VA)]¡¤5DMA.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²+80.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2557
_refine_ls_number_parameters      196
_refine_ls_number_restraints      85
_refine_ls_R_factor_all           0.1661
_refine_ls_R_factor_gt            0.1419
_refine_ls_wR_factor_ref          0.3777
_refine_ls_wR_factor_gt           0.3596
_refine_ls_goodness_of_fit_ref    1.003
_refine_ls_restrained_S_all       1.007
_refine_ls_shift/su_max           0.007
_refine_ls_shift/su_mean          0.001
 
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
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Zn1 Zn 0.05892(11) 1.0000 0.62961(16) 0.0364(10) Uani 1 2 d S T P . .
N1 N 0.1409(11) 1.0000 0.8075(17) 0.069(5) Uani 1 2 d S TU P . .
O1 O -0.0192(5) 0.9345(5) 0.6007(7) 0.071(3) Uani 1 1 d . . . . .
O2 O -0.1101(5) 0.9341(5) 0.4012(8) 0.068(3) Uani 1 1 d . . . . .
C1 C -0.0825(8) 0.9149(6) 0.4999(11) 0.043(3) Uani 1 1 d . U . . .
C2 C -0.1317(8) 0.8642(6) 0.5007(11) 0.046(3) Uani 1 1 d . . . . .
C3 C -0.2019(9) 0.8401(8) 0.3961(11) 0.079(5) Uani 1 1 d . . . . .
H3 H -0.2173 0.8517 0.3250 0.095 Uiso 1 1 calc R U . . .
C4 C -0.2476(9) 0.7993(8) 0.3996(11) 0.084(6) Uani 1 1 d . . . . .
H4 H -0.2980 0.7878 0.3289 0.100 Uiso 1 1 calc R U . . .
C5 C -0.2251(7) 0.7743(7) 0.4980(11) 0.054(4) Uani 1 1 d . . . . .
C6 C -0.1543(10) 0.7955(8) 0.6014(13) 0.081(5) Uani 1 1 d . U . . .
H6 H -0.1370 0.7806 0.6723 0.098 Uiso 1 1 calc R U . . .
C7 C -0.1068(9) 0.8413(8) 0.5992(12) 0.070(4) Uani 1 1 d . U . . .
H7 H -0.0575 0.8549 0.6694 0.084 Uiso 1 1 calc R U . . .
C8 C 0.2111(16) 1.0000 0.865(2) 0.119(9) Uani 1 2 d S TU P . .
H8 H 0.2303 1.0000 0.8260 0.142 Uiso 1 2 calc R U P . .
C9 C 0.2693(16) 1.0000 0.988(2) 0.125(9) Uani 1 2 d S TU P . .
H9 H 0.3242 1.0000 1.0263 0.151 Uiso 1 2 calc R U P . .
C10 C 0.2497(13) 1.0000 1.0469(19) 0.073(6) Uani 1 2 d S TU P . .
C11 C 0.1689(17) 1.0000 0.987(3) 0.141(11) Uani 1 2 d S TU P . .
H11 H 0.1496 1.0000 1.0260 0.169 Uiso 1 2 calc R U P . .
C12 C 0.1174(17) 1.0000 0.868(3) 0.22(3) Uani 1 2 d S T P . .
H12 H 0.0619 1.0000 0.8258 0.269 Uiso 1 2 calc R U P . .
C13 C 0.3058(18) 1.0000 1.179(2) 0.111(10) Uani 1 2 d S TU P . .
H13 H 0.2827 1.0000 1.2129 0.134 Uiso 1 2 calc R U P . .
C14 C 0.3829(19) 1.0000 1.247(2) 0.111(10) Uani 1 2 d S TU P . .
H14 H 0.4039 1.0000 1.2108 0.133 Uiso 1 2 calc R U P . .
C15 C 0.4418(14) 1.0000 1.3740(19) 0.090(8) Uani 1 2 d S T P . .
C16 C 0.4338(18) 1.0458(17) 1.438(2) 0.071(9) Uani 0.5 1 d . U P . .
C17 C 0.3649(19) 1.0852(19) 1.381(3) 0.100(13) Uani 0.5 1 d . . P . .
H17 H 0.3235 1.0820 1.3004 0.119 Uiso 0.5 1 calc R U P . .
C18 C 0.356(3) 1.130(3) 1.443(4) 0.19(3) Uani 0.5 1 d . . P . .
H18 H 0.3156 1.1614 1.4062 0.230 Uiso 0.5 1 calc R U P . .
C19 C 0.5087(19) 0.9609(16) 1.431(3) 0.077(9) Uani 0.5 1 d . U P . .
C20 C 0.516(3) 0.921(2) 1.370(4) 0.107(14) Uani 0.5 1 d . . P . .
H20 H 0.4762 0.9207 1.2889 0.129 Uiso 0.5 1 calc R U P . .
C21 C 0.581(3) 0.879(3) 1.426(4) 0.139(19) Uani 0.5 1 d . . P . .
H21 H 0.5856 0.8553 1.3793 0.167 Uiso 0.5 1 calc R U P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Zn1 O1 2.012(11) . ?
Zn1 O1 2.012(11) 6_575 ?
Zn1 O2 2.029(10) 5_576 ?
Zn1 O2 2.029(10) 2_556 ?
Zn1 N1 2.03(2) . ?
Zn1 Zn1 2.959(6) 5_576 ?
N1 C8 1.17(3) . ?
N1 C12 1.32(4) . ?
O1 C1 1.278(14) . ?
O2 C1 1.260(14) . ?
O2 Zn1 2.029(10) 5_576 ?
C1 C2 1.525(17) . ?
C2 C7 1.304(17) . ?
C2 C3 1.386(17) . ?
C3 C4 1.349(19) . ?
C3 H3 0.9300 . ?
C4 C5 1.339(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.361(18) . ?
C5 C5 1.53(2) 7_466 ?
C6 C7 1.44(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.41(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.22(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.36(3) . ?
C10 C13 1.52(3) . ?
C11 C12 1.37(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.27(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.45(3) . ?
C14 H14 0.9300 . ?
C15 C19 1.38(3) 6_575 ?
C15 C19 1.38(3) . ?
C15 C16 1.46(3) . ?
C15 C16 1.46(3) 6_575 ?
C16 C17 1.41(5) . ?
C16 C19 1.50(4) 5_678 ?
C16 C19 1.73(4) 6_575 ?
C16 C16 1.93(7) 6_575 ?
C17 C18 1.44(5) . ?
C17 H17 0.9300 . ?
C18 C21 1.52(6) 5_678 ?
C18 H18 0.9300 . ?
C19 C20 1.34(5) . ?
C19 C16 1.50(4) 5_678 ?
C19 C19 1.65(7) 6_575 ?
C19 C16 1.73(4) 6_575 ?
C20 C21 1.39(6) . ?
C20 H20 0.9300 . ?
C21 C18 1.52(6) 5_678 ?
C21 H21 0.9300 . ?
 
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
 _geom_angle_publ_flag
O1 Zn1 O1 86.4(6) . 6_575 ?
O1 Zn1 O2 160.6(4) . 5_576 ?
O1 Zn1 O2 90.5(5) 6_575 5_576 ?
O1 Zn1 O2 90.5(5) . 2_556 ?
O1 Zn1 O2 160.6(4) 6_575 2_556 ?
O2 Zn1 O2 86.2(6) 5_576 2_556 ?
O1 Zn1 N1 99.5(5) . . ?
O1 Zn1 N1 99.5(5) 6_575 . ?
O2 Zn1 N1 99.9(5) 5_576 . ?
O2 Zn1 N1 99.9(5) 2_556 . ?
O1 Zn1 Zn1 81.0(3) . 5_576 ?
O1 Zn1 Zn1 81.0(3) 6_575 5_576 ?
O2 Zn1 Zn1 79.6(3) 5_576 5_576 ?
O2 Zn1 Zn1 79.6(3) 2_556 5_576 ?
N1 Zn1 Zn1 179.3(5) . 5_576 ?
C8 N1 C12 114(2) . . ?
C8 N1 Zn1 124.3(18) . . ?
C12 N1 Zn1 121.3(17) . . ?
C1 O1 Zn1 125.1(8) . . ?
C1 O2 Zn1 126.5(8) . 5_576 ?
O2 C1 O1 127.7(12) . . ?
O2 C1 C2 116.9(11) . . ?
O1 C1 C2 115.4(11) . . ?
C7 C2 C3 119.1(12) . . ?
C7 C2 C1 120.7(12) . . ?
C3 C2 C1 120.2(11) . . ?
C4 C3 C2 118.6(12) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 124.3(12) . . ?
C5 C4 H4 117.8 . . ?
C3 C4 H4 117.8 . . ?
C4 C5 C6 117.3(12) . . ?
C4 C5 C5 124.5(14) . 7_466 ?
C6 C5 C5 118.2(14) . 7_466 ?
C5 C6 C7 118.8(13) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C2 C7 C6 121.3(13) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
N1 C8 C9 125(2) . . ?
N1 C8 H8 117.3 . . ?
C9 C8 H8 117.3 . . ?
C10 C9 C8 122(3) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C9 C10 C11 117(3) . . ?
C9 C10 C13 127(2) . . ?
C11 C10 C13 116(2) . . ?
C10 C11 C12 117(3) . . ?
C10 C11 H11 121.6 . . ?
C12 C11 H11 121.6 . . ?
N1 C12 C11 125(3) . . ?
N1 C12 H12 117.7 . . ?
C11 C12 H12 117.7 . . ?
C14 C13 C10 123(2) . . ?
C14 C13 H13 118.4 . . ?
C10 C13 H13 118.4 . . ?
C13 C14 C15 128(3) . . ?
C13 C14 H14 116.1 . . ?
C15 C14 H14 116.1 . . ?
C19 C15 C19 73(3) 6_575 . ?
C19 C15 C14 119(2) 6_575 . ?
C19 C15 C14 119(2) . . ?
C19 C15 C16 74.7(19) 6_575 . ?
C19 C15 C16 121(2) . . ?
C14 C15 C16 119.7(19) . . ?
C19 C15 C16 121(2) 6_575 6_575 ?
C19 C15 C16 74.7(19) . 6_575 ?
C14 C15 C16 119.7(19) . 6_575 ?
C16 C15 C16 82(3) . 6_575 ?
C17 C16 C15 122(2) . . ?
C17 C16 C19 119(3) . 5_678 ?
C15 C16 C19 117(3) . 5_678 ?
C17 C16 C19 134(3) . 6_575 ?
C15 C16 C19 50.4(16) . 6_575 ?
C19 C16 C19 94(2) 5_678 6_575 ?
C17 C16 C16 126(2) . 6_575 ?
C15 C16 C16 48.9(14) . 6_575 ?
C19 C16 C16 84.6(19) 5_678 6_575 ?
C19 C16 C16 85.3(16) 6_575 6_575 ?
C16 C17 C18 123(3) . . ?
C16 C17 H17 118.5 . . ?
C18 C17 H17 118.5 . . ?
C17 C18 C21 112(4) . 5_678 ?
C17 C18 H18 124.0 . . ?
C21 C18 H18 124.1 5_678 . ?
C20 C19 C15 120(3) . . ?
C20 C19 C16 119(3) . 5_678 ?
C15 C19 C16 120(3) . 5_678 ?
C20 C19 C19 129(2) . 6_575 ?
C15 C19 C19 53.4(15) . 6_575 ?
C16 C19 C19 95.4(19) 5_678 6_575 ?
C20 C19 C16 123(3) . 6_575 ?
C15 C19 C16 54.9(16) . 6_575 ?
C16 C19 C16 85(2) 5_678 6_575 ?
C19 C19 C16 94.7(16) 6_575 6_575 ?
C19 C20 C21 122(4) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C18 124(4) . 5_678 ?
C20 C21 H21 117.9 . . ?
C18 C21 H21 117.9 5_678 . ?
 
_refine_diff_density_max    1.579
_refine_diff_density_min   -0.928
_refine_diff_density_rms    0.126




