#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:40:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180191 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/87/7108735.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_7108735
loop_
_publ_author_name
'Lei Han'
'Lan Qin'
'Lanping Xu'
'Yan Zhou'
'Junliang Sun'
'Xiaodong Zou'
_publ_section_title
;
 A novel photochromic calcium-based metal-organic framework derived from a
 naphthalene diimide chromophore
;
_journal_name_full               Chem.Commun.
_journal_page_first              406
_journal_paper_doi               10.1039/c2cc37497h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C21 H19 Ca N3 O8, C3 H7 N O '
_chemical_formula_sum            'C24 H26 Ca N4 O9'
_chemical_formula_weight         554.57
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   28.2810(8)
_cell_length_b                   28.2810(8)
_cell_length_c                   13.5488(7)
_cell_measurement_temperature    298(2)
_cell_volume                     10836.5(7)
_computing_cell_refinement       'SMART '
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_sigmaI/netI    0.1610
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            37248
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.67
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4640
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5502
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0648P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                2657
_reflns_number_total             5502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37497h.txt
_cod_data_source_block           sun3
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7108735
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'
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
Ca1 Ca 0.19023(3) -0.00490(4) 0.62304(9) 0.0280(2) Uani 1 1 d .
O1 O 0.20341(12) 0.00244(13) 0.4239(3) 0.0404(10) Uani 1 1 d .
O2 O 0.16589(13) 0.05590(14) 0.5102(3) 0.0475(11) Uani 1 1 d .
O3 O 0.24182(13) 0.04691(12) 0.0685(2) 0.0344(9) Uani 1 1 d .
O4 O 0.18158(13) 0.07738(14) -0.0121(3) 0.0453(10) Uani 1 1 d .
O5 O 0.14404(17) 0.21669(14) 0.2600(4) 0.0748(15) Uani 1 1 d .
O6 O 0.02956(15) 0.10554(17) 0.2595(4) 0.0839(17) Uani 1 1 d .
O7 O 0.13003(16) -0.05118(18) 0.5376(3) 0.0701(14) Uani 1 1 d .
O8 O 0.12285(17) 0.03137(18) 0.7040(3) 0.0736(15) Uani 1 1 d .
N1 N 0.08709(17) 0.16164(17) 0.2550(4) 0.0376(10) Uani 1 1 d .
N2 N 0.0877(3) -0.0330(3) 0.3959(6) 0.123(3) Uani 1 1 d .
N3 N 0.0778(2) 0.0117(2) 0.8382(4) 0.0665(16) Uani 1 1 d .
C1 C 0.18026(18) 0.04020(19) 0.4305(4) 0.0335(13) Uani 1 1 d .
C2 C 0.20148(18) 0.06617(17) 0.0652(4) 0.0284(12) Uani 1 1 d .
C3 C 0.16854(17) 0.06609(18) 0.3382(4) 0.0295(12) Uani 1 1 d .
C4 C 0.19091(18) 0.05451(17) 0.2482(4) 0.0292(11) Uani 1 1 d .
H4A H 0.2148 0.0309 0.2468 0.035 Uiso 1 1 calc R
C5 C 0.17798(18) 0.07755(17) 0.1613(4) 0.0310(13) Uani 1 1 d .
C6 C 0.14273(19) 0.11169(19) 0.1648(4) 0.0361(14) Uani 1 1 d .
H6A H 0.1323 0.1265 0.1058 0.043 Uiso 1 1 calc R
C7 C 0.12284(19) 0.1241(2) 0.2545(4) 0.0374(13) Uani 1 1 d .
C8 C 0.13483(19) 0.10175(18) 0.3402(4) 0.0337(13) Uani 1 1 d .
H8A H 0.1202 0.1105 0.4006 0.040 Uiso 1 1 calc R
C9 C 0.1024(2) 0.2078(2) 0.2582(4) 0.0401(15) Uani 1 1 d .
C10 C 0.0394(2) 0.1466(2) 0.2586(5) 0.0468(17) Uani 1 1 d .
C11 C -0.0439(2) 0.1731(2) 0.2612(5) 0.0591(19) Uani 1 1 d .
H11A H -0.0535 0.1410 0.2645 0.071 Uiso 1 1 calc R
C12 C 0.00357(19) 0.18476(19) 0.2587(4) 0.0390(15) Uani 1 1 d .
C13 C 0.0777(2) 0.2909(2) 0.2587(5) 0.0582(19) Uani 1 1 d .
H13A H 0.1102 0.2992 0.2572 0.070 Uiso 1 1 calc R
C14 C 0.0658(2) 0.2441(2) 0.2584(4) 0.0412(16) Uani 1 1 d .
C15 C 0.0181(2) 0.2321(2) 0.2575(4) 0.0347(12) Uani 1 1 d .
C16 C 0.1219(3) -0.0569(3) 0.4493(7) 0.089(2) Uani 1 1 d .
H16A H 0.1405 -0.0796 0.4150 0.107 Uiso 1 1 calc R
C17 C 0.0576(3) 0.0019(4) 0.4409(8) 0.144(5) Uani 1 1 d .
H17A H 0.0643 0.0035 0.5118 0.216 Uiso 1 1 calc R
H17B H 0.0245 -0.0069 0.4307 0.216 Uiso 1 1 calc R
H17C H 0.0636 0.0329 0.4109 0.216 Uiso 1 1 calc R
C18 C 0.0812(4) -0.0377(4) 0.2893(6) 0.141(5) Uani 1 1 d .
H18A H 0.0546 -0.0179 0.2681 0.211 Uiso 1 1 calc R
H18B H 0.0745 -0.0709 0.2732 0.211 Uiso 1 1 calc R
H18C H 0.1100 -0.0277 0.2552 0.211 Uiso 1 1 calc R
C19 C 0.1116(3) 0.0358(2) 0.7910(6) 0.067(2) Uani 1 1 d .
H19A H 0.1286 0.0585 0.8285 0.081 Uiso 1 1 calc R
C20 C 0.0521(3) -0.0235(3) 0.7874(7) 0.118(4) Uani 1 1 d .
H20A H 0.0681 -0.0309 0.7251 0.177 Uiso 1 1 calc R
H20B H 0.0201 -0.0119 0.7737 0.177 Uiso 1 1 calc R
H20C H 0.0503 -0.0520 0.8282 0.177 Uiso 1 1 calc R
C21 C 0.0676(2) 0.0209(3) 0.9414(4) 0.109(3) Uani 1 1 d .
H21A H 0.0917 0.0422 0.9685 0.163 Uiso 1 1 calc R
H21B H 0.0680 -0.0090 0.9781 0.163 Uiso 1 1 calc R
H21C H 0.0364 0.0356 0.9473 0.163 Uiso 1 1 calc R
O31 O 0.0583(2) 0.1882(3) 0.4755(4) 0.280(7) Uani 1 1 d R
N31 N 0.0530(2) 0.1523(3) 0.6232(4) 0.478(16) Uani 1 1 d RDU
C31 C 0.0447(2) 0.1052(3) 0.5862(4) 0.432(10) Uani 1 1 d RU
H31A H 0.0384 0.0838 0.6416 0.648 Uiso 1 1 calc R
H31B H 0.0726 0.0943 0.5501 0.648 Uiso 1 1 calc R
H31C H 0.0173 0.1056 0.5417 0.648 Uiso 1 1 calc R
C32 C 0.0598(2) 0.1610(3) 0.7264(4) 0.432(10) Uani 1 1 d RD
H32A H 0.0521 0.1323 0.7638 0.648 Uiso 1 1 calc R
H32B H 0.0393 0.1869 0.7476 0.648 Uiso 1 1 calc R
H32C H 0.0929 0.1695 0.7384 0.648 Uiso 1 1 calc R
C33 C 0.0622(2) 0.1877(3) 0.5659(4) 0.432(10) Uani 1 1 d R
H33 H 0.0729 0.2160 0.5965 0.518 Uiso 1 1 calc R
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'
Ca Ca 0.2262 0.3064 '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'
H H 0.0000 0.0000 '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
O3 Ca1 O1 78.38(10) 7_545 4
O3 Ca1 O2 113.06(12) 7_545 .
O1 Ca1 O2 87.60(13) 4 .
O3 Ca1 O8 170.67(14) 7_545 .
O1 Ca1 O8 101.00(15) 4 .
O2 Ca1 O8 76.11(14) . .
O3 Ca1 O4 89.72(13) 7_545 6_445
O1 Ca1 O4 114.70(13) 4 6_445
O2 Ca1 O4 151.50(13) . 6_445
O8 Ca1 O4 82.07(16) . 6_445
O3 Ca1 O7 98.55(15) 7_545 .
O1 Ca1 O7 168.31(14) 4 .
O2 Ca1 O7 83.23(16) . .
O8 Ca1 O7 83.86(16) . .
O4 Ca1 O7 76.34(14) 6_445 .
O3 Ca1 O3 100.39(11) 7_545 6_445
O1 Ca1 O3 68.59(11) 4 6_445
O2 Ca1 O3 133.96(13) . 6_445
O8 Ca1 O3 70.97(13) . 6_445
O4 Ca1 O3 50.79(12) 6_445 6_445
O7 Ca1 O3 123.09(13) . 6_445
O3 Ca1 O1 67.71(10) 7_545 .
O1 Ca1 O1 97.94(11) 4 .
O2 Ca1 O1 49.90(11) . .
O8 Ca1 O1 121.44(13) . .
O4 Ca1 O1 135.82(13) 6_445 .
O7 Ca1 O1 70.58(12) . .
O3 Ca1 O1 164.16(9) 6_445 .
O3 Ca1 C2 96.74(13) 7_545 6_445
O1 Ca1 C2 92.68(14) 4 6_445
O2 Ca1 C2 149.56(14) . 6_445
O8 Ca1 C2 73.96(15) . 6_445
O4 Ca1 C2 24.91(12) 6_445 6_445
O7 Ca1 C2 98.90(15) . 6_445
O3 Ca1 C2 25.94(12) 6_445 6_445
O1 Ca1 C2 158.72(14) . 6_445
O3 Ca1 C1 91.07(14) 7_545 .
O1 Ca1 C1 93.59(14) 4 .
O2 Ca1 C1 24.51(12) . .
O8 Ca1 C1 98.25(16) . .
O4 Ca1 C1 151.23(15) 6_445 .
O7 Ca1 C1 75.10(15) . .
O3 Ca1 C1 156.01(14) 6_445 .
O1 Ca1 C1 25.41(12) . .
C2 Ca1 C1 170.83(13) 6_445 .
O3 Ca1 Ca1 99.88(9) 7_545 4
O1 Ca1 Ca1 38.71(9) 4 4
O2 Ca1 Ca1 108.14(10) . 4
O8 Ca1 Ca1 74.84(12) . 4
O4 Ca1 Ca1 83.09(9) 6_445 4
O7 Ca1 Ca1 152.19(11) . 4
O3 Ca1 Ca1 32.48(8) 6_445 4
O1 Ca1 Ca1 136.19(8) . 4
C2 Ca1 Ca1 58.38(11) 6_445 4
C1 Ca1 Ca1 124.98(11) . 4
O3 Ca1 Ca1 37.18(9) 7_545 6_444
O1 Ca1 Ca1 97.98(8) 4 6_444
O2 Ca1 Ca1 82.79(9) . 6_444
O8 Ca1 Ca1 150.82(12) . 6_444
O4 Ca1 Ca1 109.67(11) 6_445 6_444
O7 Ca1 Ca1 73.73(11) . 6_444
O3 Ca1 Ca1 137.32(8) 6_445 6_444
O1 Ca1 Ca1 33.09(8) . 6_444
C2 Ca1 Ca1 127.15(11) 6_445 6_444
C1 Ca1 Ca1 58.42(11) . 6_444
Ca1 Ca1 Ca1 131.761(19) 4 6_444
C1 O1 Ca1 165.0(3) . 6_444
C1 O1 Ca1 85.6(3) . .
Ca1 O1 Ca1 108.20(13) 6_444 .
C1 O2 Ca1 101.8(3) . .
C2 O3 Ca1 162.8(3) . 7_544
C2 O3 Ca1 86.4(3) . 4_554
Ca1 O3 Ca1 110.34(13) 7_544 4_554
C2 O4 Ca1 98.9(3) . 4_554
C16 O7 Ca1 131.5(5) . .
C19 O8 Ca1 132.9(4) . .
C9 N1 C10 125.8(4) . .
C9 N1 C7 118.1(5) . .
C10 N1 C7 116.0(5) . .
C16 N2 C17 121.8(8) . .
C16 N2 C18 124.0(9) . .
C17 N2 C18 114.1(9) . .
C19 N3 C20 119.7(7) . .
C19 N3 C21 120.7(7) . .
C20 N3 C21 119.6(7) . .
O2 C1 O1 122.6(5) . .
O2 C1 C3 119.0(5) . .
O1 C1 C3 118.4(5) . .
O2 C1 Ca1 53.7(3) . .
O1 C1 Ca1 69.0(3) . .
C3 C1 Ca1 171.5(4) . .
O4 C2 O3 123.6(4) . .
O4 C2 C5 118.8(4) . .
O3 C2 C5 117.5(4) . .
O4 C2 Ca1 56.2(2) . 4_554
O3 C2 Ca1 67.6(3) . 4_554
C5 C2 Ca1 171.0(3) . 4_554
C8 C3 C4 119.5(4) . .
C8 C3 C1 119.7(5) . .
C4 C3 C1 120.8(4) . .
C5 C4 C3 120.2(4) . .
C6 C5 C4 118.9(5) . .
C6 C5 C2 119.9(5) . .
C4 C5 C2 121.2(4) . .
C7 C6 C5 119.9(5) . .
C8 C7 C6 122.0(4) . .
C8 C7 N1 120.2(5) . .
C6 C7 N1 117.9(5) . .
C7 C8 C3 119.4(5) . .
O5 C9 N1 120.5(5) . .
O5 C9 C14 123.1(6) . .
N1 C9 C14 116.4(5) . .
O6 C10 N1 121.0(5) . .
O6 C10 C12 123.4(6) . .
N1 C10 C12 115.6(5) . .
C12 C11 C13 119.3(7) . 3
C11 C12 C15 120.8(5) . .
C11 C12 C10 119.4(5) . .
C15 C12 C10 119.8(5) . .
C14 C13 C11 122.7(6) . 3
C13 C14 C15 118.3(5) . .
C13 C14 C9 120.5(6) . .
C15 C14 C9 121.1(5) . .
C14 C15 C12 121.1(4) . .
C14 C15 C15 121.2(7) . 3
C12 C15 C15 117.7(7) . 3
O7 C16 N2 125.0(9) . .
O8 C19 N3 126.3(7) . .
C33 N31 C32 115.2 . .
C33 N31 C31 122.6 . .
C32 N31 C31 121.2 . .
O31 C33 N31 126.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O3 2.377(4) 7_545
Ca1 O1 2.385(4) 4
Ca1 O2 2.402(4) .
Ca1 O8 2.426(4) .
Ca1 O4 2.428(4) 6_445
Ca1 O7 2.439(5) .
Ca1 O3 2.675(3) 6_445
Ca1 O1 2.732(4) .
Ca1 C2 2.887(5) 6_445
Ca1 C1 2.917(5) .
Ca1 Ca1 4.1505(8) 4
Ca1 Ca1 4.1505(8) 6_444
O1 C1 1.256(6) .
O1 Ca1 2.385(4) 6_444
O2 C1 1.236(6) .
O3 C2 1.265(6) .
O3 Ca1 2.377(4) 7_544
O3 Ca1 2.675(3) 4_554
O4 C2 1.230(6) .
O4 Ca1 2.428(4) 4_554
O5 C9 1.204(7) .
O6 C10 1.193(7) .
O7 C16 1.230(9) .
O8 C19 1.228(8) .
N1 C9 1.375(7) .
N1 C10 1.416(7) .
N1 C7 1.467(6) .
N2 C16 1.385(11) .
N2 C17 1.438(11) .
N2 C18 1.462(10) .
N3 C19 1.337(9) .
N3 C20 1.411(9) .
N3 C21 1.451(8) .
C1 C3 1.487(7) .
C2 C5 1.497(6) .
C2 Ca1 2.887(5) 4_554
C3 C8 1.388(7) .
C3 C4 1.413(6) .
C4 C5 1.395(6) .
C5 C6 1.389(7) .
C6 C7 1.383(7) .
C7 C8 1.364(7) .
C9 C14 1.459(8) .
C10 C12 1.481(8) .
C11 C12 1.384(9) .
C11 C13 1.396(8) 3
C12 C15 1.400(8) .
C13 C14 1.365(8) .
C13 C11 1.396(8) 3
C14 C15 1.391(8) .
C15 C15 1.438(9) 3
O31 C33 1.2302 .
N31 C33 1.2933 .
N31 C32 1.4327 .
N31 C31 1.4425 .
