#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:20:56 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180501 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/70/7217075.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_7217075
loop_
_publ_author_name
'Yang, De-Liang'
'Zhang, Xin'
'Yao, Yuan-Gen'
'Zhang, Jian'
_publ_section_title
;
 Structure versatility of coordination polymers constructed from a
 semirigid ligand and polynuclear metal clusters
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              8047
_journal_paper_doi               10.1039/C4CE01032A
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C16 H6 Cd O9, 2(C4 H9 N O), Ca '
_chemical_formula_sum            'C24 H24 Ca Cd N2 O11'
_chemical_formula_weight         668.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.389(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0047(7)
_cell_length_b                   10.9563(7)
_cell_length_c                   21.0767(15)
_cell_measurement_reflns_used    2896
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0305
_cell_measurement_theta_min      2.5607
_cell_volume                     2659.5(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'multiwire proportional'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6968
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4324
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0303P)²+2.7095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                3617
_reflns_number_total             4683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce01032a2.cif
_cod_data_source_block           Compound-2
_cod_depositor_comments
'Adding full bibliography for 7217074--7217078.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7217075
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Cd1 Cd 0.63605(2) 1.68064(3) -0.039712(14) 0.02231(11) Uani 1 1 d .
Ca2 Ca 0.35622(6) 1.55455(8) -0.12728(4) 0.0217(2) Uani 1 1 d .
O1 O 0.6272(2) 1.7688(3) -0.13490(14) 0.0336(8) Uani 1 1 d .
O2 O 0.4381(2) 1.7243(3) -0.16496(15) 0.0339(8) Uani 1 1 d .
O3 O 0.2204(2) 1.8812(3) -0.40912(15) 0.0345(8) Uani 1 1 d .
O4 O 0.3097(2) 1.7736(3) -0.46972(14) 0.0342(8) Uani 1 1 d .
O5 O 0.7319(2) 1.8495(3) -0.34110(15) 0.0341(8) Uani 1 1 d .
O6 O 0.9634(2) 1.9686(3) -0.39303(16) 0.0413(9) Uani 1 1 d .
O7 O 0.7819(3) 2.0004(3) -0.45050(17) 0.0412(8) Uani 1 1 d .
O8 O 1.0417(3) 1.6771(3) -0.49329(16) 0.0391(8) Uani 1 1 d .
O9 O 0.9441(3) 1.8487(3) -0.52188(15) 0.0329(7) Uani 1 1 d .
O10 O 0.3144(3) 1.4925(4) -0.23725(17) 0.0612(11) Uani 1 1 d .
O11 O 0.1819(3) 1.6488(4) -0.1385(2) 0.0688(13) Uani 1 1 d .
N1 N 0.3842(11) 1.4840(6) -0.3233(4) 0.149(4) Uani 1 1 d .
N2 N 0.0087(4) 1.6584(5) -0.1236(3) 0.0718(17) Uani 1 1 d .
C1 C 0.5283(3) 1.7624(4) -0.1764(2) 0.0238(9) Uani 1 1 d .
C2 C 0.5227(3) 1.7997(4) -0.24616(19) 0.0206(9) Uani 1 1 d .
C3 C 0.4188(3) 1.8068(4) -0.2959(2) 0.0228(9) Uani 1 1 d .
H3A H 0.3489 1.8005 -0.2854 0.027 Uiso 1 1 calc R
C4 C 0.4182(3) 1.8231(4) -0.36094(19) 0.0232(9) Uani 1 1 d .
C5 C 0.5231(3) 1.8329(4) -0.3768(2) 0.0274(10) Uani 1 1 d .
H5A H 0.5234 1.8399 -0.4207 0.033 Uiso 1 1 calc R
C6 C 0.6258(3) 1.8322(4) -0.3272(2) 0.0253(10) Uani 1 1 d .
C7 C 0.6273(3) 1.8165(4) -0.2618(2) 0.0243(9) Uani 1 1 d .
H7A H 0.6973 1.8170 -0.2286 0.029 Uiso 1 1 calc R
C8 C 0.3078(4) 1.8259(4) -0.4170(2) 0.0273(10) Uani 1 1 d .
C9 C 0.7656(3) 1.7604(4) -0.3787(2) 0.0286(10) Uani 1 1 d .
C10 C 0.8363(3) 1.7986(4) -0.4171(2) 0.0224(9) Uani 1 1 d .
C11 C 0.8816(3) 1.7111(4) -0.4507(2) 0.0294(11) Uani 1 1 d .
C12 C 0.8574(4) 1.5881(5) -0.4454(3) 0.0438(13) Uani 1 1 d .
H12A H 0.8903 1.5298 -0.4667 0.053 Uiso 1 1 calc R
C13 C 0.7841(4) 1.5526(5) -0.4083(3) 0.0545(16) Uani 1 1 d .
H13A H 0.7657 1.4706 -0.4061 0.065 Uiso 1 1 calc R
C14 C 0.7384(4) 1.6383(5) -0.3747(3) 0.0434(13) Uani 1 1 d .
H14A H 0.6897 1.6142 -0.3497 0.052 Uiso 1 1 calc R
C15 C 0.8628(4) 1.9320(4) -0.4205(2) 0.0268(10) Uani 1 1 d .
C16 C 0.9596(4) 1.7470(4) -0.4916(2) 0.0285(10) Uani 1 1 d .
C17 C 0.1783(6) 1.5015(8) -0.3491(3) 0.099(3) Uani 1 1 d .
H17A H 0.1831 1.4997 -0.3938 0.149 Uiso 1 1 calc RD
H17B H 0.1430 1.5767 -0.3415 0.149 Uiso 1 1 calc R
H17C H 0.1321 1.4341 -0.3420 0.149 Uiso 1 1 calc R
C18 C 0.3141(9) 1.4911(6) -0.2959(5) 0.100(3) Uani 1 1 d .
C19 C 0.3899(8) 1.4846(8) -0.3937(4) 0.123(3) Uani 1 1 d .
H19A H 0.3127 1.4884 -0.4232 0.184 Uiso 1 1 calc RD
H19B H 0.4274 1.4114 -0.4022 0.184 Uiso 1 1 calc R
H19C H 0.4334 1.5544 -0.4008 0.184 Uiso 1 1 calc R
C20 C 0.5092(6) 1.4786(7) -0.2710(4) 0.085(2) Uani 1 1 d .
H20A H 0.5010 1.4788 -0.2270 0.128 Uiso 1 1 calc R
H20B H 0.5538 1.5483 -0.2768 0.128 Uiso 1 1 calc R
H20C H 0.5483 1.4053 -0.2778 0.128 Uiso 1 1 calc R
C21 C 0.0742(5) 1.6518(5) -0.1612(3) 0.0575(16) Uani 1 1 d .
C22 C 0.0181(7) 1.6464(7) -0.2357(3) 0.097(3) Uani 1 1 d .
H22A H 0.0775 1.6416 -0.2580 0.146 Uiso 1 1 calc R
H22B H -0.0276 1.7185 -0.2497 0.146 Uiso 1 1 calc R
H22C H -0.0308 1.5757 -0.2462 0.146 Uiso 1 1 calc R
C23 C 0.0652(7) 1.6581(8) -0.0503(3) 0.098(3) Uani 1 1 d .
H23A H 0.1481 1.6574 -0.0419 0.147 Uiso 1 1 calc R
H23B H 0.0413 1.5869 -0.0311 0.147 Uiso 1 1 calc R
H23C H 0.0424 1.7300 -0.0310 0.147 Uiso 1 1 calc R
C24 C -0.1184(5) 1.6604(7) -0.1447(5) 0.106(3) Uani 1 1 d .
H24A H -0.1454 1.6603 -0.1922 0.159 Uiso 1 1 calc R
H24B H -0.1456 1.7326 -0.1280 0.159 Uiso 1 1 calc R
H24C H -0.1476 1.5895 -0.1279 0.159 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'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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 Cd1 O7 102.22(12) . 2_644
O1 Cd1 O4 107.33(11) . 4_696
O7 Cd1 O4 84.63(12) 2_644 4_696
O1 Cd1 O8 100.82(12) . 4_596
O7 Cd1 O8 156.55(12) 2_644 4_596
O4 Cd1 O8 92.68(12) 4_696 4_596
O1 Cd1 O9 112.99(10) . 4_596
O7 Cd1 O9 110.74(11) 2_644 4_596
O4 Cd1 O9 131.73(10) 4_696 4_596
O8 Cd1 O9 55.13(10) 4_596 4_596
O1 Cd1 C16 111.75(12) . 4_596
O7 Cd1 C16 134.57(13) 2_644 4_596
O4 Cd1 C16 111.57(12) 4_696 4_596
O8 Cd1 C16 27.48(12) 4_596 4_596
O9 Cd1 C16 27.92(12) 4_596 4_596
O1 Cd1 Ca2 84.47(8) . .
O7 Cd1 Ca2 89.18(8) 2_644 .
O4 Cd1 Ca2 167.59(8) 4_696 .
O8 Cd1 Ca2 88.73(8) 4_596 .
O9 Cd1 Ca2 41.66(7) 4_596 .
C16 Cd1 Ca2 65.90(10) 4_596 .
O11 Ca2 O6 174.86(15) . 2_644
O11 Ca2 O10 95.44(16) . .
O6 Ca2 O10 89.58(14) 2_644 .
O11 Ca2 O3 88.13(13) . 2_544
O6 Ca2 O3 92.49(12) 2_644 2_544
O10 Ca2 O3 95.47(13) . 2_544
O11 Ca2 O2 93.79(13) . .
O6 Ca2 O2 85.67(12) 2_644 .
O10 Ca2 O2 83.55(13) . .
O3 Ca2 O2 177.92(12) 2_544 .
O11 Ca2 O9 92.68(14) . 4_596
O6 Ca2 O9 82.19(11) 2_644 4_596
O10 Ca2 O9 163.18(12) . 4_596
O3 Ca2 O9 99.50(11) 2_544 4_596
O2 Ca2 O9 81.23(11) . 4_596
O11 Ca2 Cd1 124.86(11) . .
O6 Ca2 Cd1 50.85(9) 2_644 .
O10 Ca2 Cd1 121.80(10) . .
O3 Ca2 Cd1 122.58(7) 2_544 .
O2 Ca2 Cd1 56.79(7) . .
O9 Ca2 Cd1 42.50(7) 4_596 .
C1 O1 Cd1 113.6(3) . .
C1 O2 Ca2 143.3(3) . .
C8 O3 Ca2 148.6(3) . 2_554
C8 O4 Cd1 103.5(2) . 4_595
C9 O5 C6 117.0(3) . .
C15 O6 Ca2 163.6(3) . 2_654
C15 O7 Cd1 106.0(3) . 2_654
C16 O8 Cd1 94.8(3) . 4_695
C16 O9 Ca2 144.0(3) . 4_695
C16 O9 Cd1 87.2(2) . 4_695
Ca2 O9 Cd1 95.84(10) 4_695 4_695
C18 O10 Ca2 159.7(5) . .
C21 O11 Ca2 150.8(4) . .
C18 N1 C19 137.6(13) . .
C18 N1 C20 109.6(9) . .
C19 N1 C20 112.7(8) . .
C21 N2 C24 126.1(7) . .
C21 N2 C23 117.6(5) . .
C24 N2 C23 116.2(6) . .
O2 C1 O1 125.8(4) . .
O2 C1 C2 118.4(4) . .
O1 C1 C2 115.7(4) . .
C3 C2 C7 119.3(4) . .
C3 C2 C1 122.4(4) . .
C7 C2 C1 118.0(3) . .
C4 C3 C2 120.7(4) . .
C4 C3 H3A 119.7 . .
C2 C3 H3A 119.7 . .
C3 C4 C5 119.7(4) . .
C3 C4 C8 122.6(4) . .
C5 C4 C8 117.7(4) . .
C6 C5 C4 119.7(4) . .
C6 C5 H5A 120.2 . .
C4 C5 H5A 120.2 . .
C5 C6 C7 121.0(4) . .
C5 C6 O5 121.1(4) . .
C7 C6 O5 117.9(4) . .
C6 C7 C2 119.4(4) . .
C6 C7 H7A 120.3 . .
C2 C7 H7A 120.3 . .
O4 C8 O3 124.0(4) . .
O4 C8 C4 116.9(4) . .
O3 C8 C4 119.1(4) . .
C14 C9 O5 122.3(4) . .
C14 C9 C10 121.2(4) . .
O5 C9 C10 116.4(4) . .
C11 C10 C9 118.7(4) . .
C11 C10 C15 121.8(4) . .
C9 C10 C15 119.5(4) . .
C12 C11 C10 120.5(4) . .
C12 C11 C16 118.7(4) . .
C10 C11 C16 120.8(4) . .
C13 C12 C11 119.8(5) . .
C13 C12 H12A 120.1 . .
C11 C12 H12A 120.1 . .
C14 C13 C12 120.4(5) . .
C14 C13 H13A 119.8 . .
C12 C13 H13A 119.8 . .
C13 C14 C9 119.5(4) . .
C13 C14 H14A 120.3 . .
C9 C14 H14A 120.3 . .
O6 C15 O7 123.7(4) . .
O6 C15 C10 118.7(4) . .
O7 C15 C10 117.5(4) . .
O8 C16 O9 121.7(4) . .
O8 C16 C11 118.7(4) . .
O9 C16 C11 119.5(4) . .
O8 C16 Cd1 57.8(2) . 4_695
O9 C16 Cd1 64.9(2) . 4_695
C11 C16 Cd1 167.3(3) . 4_695
C18 C17 H17A 109.5 . .
C18 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C18 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
N1 C18 O10 135.0(12) . .
N1 C18 C17 112.0(10) . .
O10 C18 C17 113.0(7) . .
N1 C19 H19A 109.5 . .
N1 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
N1 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
N1 C20 H20A 109.5 . .
N1 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
N1 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
O11 C21 N2 121.4(6) . .
O11 C21 C22 120.2(6) . .
N2 C21 C22 118.4(6) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
N2 C23 H23A 109.5 . .
N2 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
N2 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N2 C24 H24A 109.5 . .
N2 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
N2 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O1 2.202(3) .
Cd1 O7 2.242(3) 2_644
Cd1 O4 2.245(3) 4_696
Cd1 O8 2.301(3) 4_596
Cd1 O9 2.458(3) 4_596
Cd1 C16 2.711(4) 4_596
Cd1 Ca2 3.6195(8) .
Ca2 O11 2.285(3) .
Ca2 O6 2.289(3) 2_644
Ca2 O10 2.330(4) .
Ca2 O3 2.333(3) 2_544
Ca2 O2 2.345(3) .
Ca2 O9 2.419(3) 4_596
O1 C1 1.262(5) .
O2 C1 1.245(5) .
O3 C8 1.262(5) .
O3 Ca2 2.333(3) 2_554
O4 C8 1.255(5) .
O4 Cd1 2.245(3) 4_595
O5 C9 1.387(5) .
O5 C6 1.398(4) .
O6 C15 1.248(5) .
O6 Ca2 2.289(3) 2_654
O7 C15 1.249(5) .
O7 Cd1 2.242(3) 2_654
O8 C16 1.255(5) .
O8 Cd1 2.301(3) 4_695
O9 C16 1.271(5) .
O9 Ca2 2.419(3) 4_695
O9 Cd1 2.458(3) 4_695
O10 C18 1.234(8) .
O11 C21 1.246(6) .
N1 C18 1.150(9) .
N1 C19 1.506(9) .
N1 C20 1.592(12) .
N2 C21 1.266(7) .
N2 C24 1.465(7) .
N2 C23 1.502(8) .
C1 C2 1.510(5) .
C2 C3 1.387(5) .
C2 C7 1.398(5) .
C3 C4 1.379(6) .
C3 H3A 0.9300 .
C4 C5 1.395(5) .
C4 C8 1.507(5) .
C5 C6 1.373(6) .
C5 H5A 0.9300 .
C6 C7 1.384(6) .
C7 H7A 0.9300 .
C9 C14 1.385(7) .
C9 C10 1.393(6) .
C10 C11 1.391(6) .
C10 C15 1.502(6) .
C11 C12 1.390(6) .
C11 C16 1.494(6) .
C12 C13 1.388(6) .
C12 H12A 0.9300 .
C13 C14 1.379(7) .
C13 H13A 0.9300 .
C14 H14A 0.9300 .
C16 Cd1 2.711(4) 4_695
C17 C18 1.703(11) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 C22 1.524(9) .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
