#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:47:15 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179596 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/60/4506022.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_4506022
loop_
_publ_author_name
'Plonka, Anna M.'
'Banerjee, Debasis'
'Parise, John B.'
_publ_section_title
;
 Effect of Ligand Structural Isomerism in Formation of Calcium
 Coordination Networks
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2460
_journal_paper_doi               10.1021/cg300093h
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C7 H3 Ca N O4'
_chemical_formula_weight         205.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   18.5021(5)
_cell_length_b                   18.5021(5)
_cell_length_c                   11.9010(4)
_cell_measurement_reflns_used    7154
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.9634
_cell_measurement_theta_min      3.6452
_cell_volume                     3528.22(18)
_computing_cell_refinement
;
CrysAlisPro 
;
_computing_data_collection
;
CrysAlisPro, (Oxford Diffraction Ltd.2010)
;
_computing_data_reduction
;
CrysAlisPro
;
_computing_molecular_graphics
;
'ORTEP-3 for Windows (Burnett & Johnson, 1996) 
and CrystalMaker (CrystalMaker, 2009)'
;
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4962
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14627
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         3.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.8602
_exptl_absorpt_correction_T_min  0.7465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro (Oxford Diffraction, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0239
_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)+(0.0367P)²+2.8700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                1420
_reflns_number_total             1603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300093h_si_002.cif
_cod_data_source_block           Ca2_6PDC
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4506022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.93959(9) 0.66759(9) 0.31214(12) 0.0193(3) Uani 1 1 d .
C2 C 1.00999(9) 0.75468(9) 0.33714(13) 0.0208(3) Uani 1 1 d .
C3 C 1.05749(10) 0.77434(11) 0.43365(14) 0.0323(4) Uani 1 1 d .
H3 H 1.0496 0.7331 0.4849 0.039 Uiso 1 1 calc R
C4 C 1.11703(12) 0.85685(12) 0.45228(16) 0.0441(5) Uani 1 1 d .
H4 H 1.1474 0.8726 0.5188 0.053 Uiso 1 1 calc R
C5 C 1.13077(11) 0.91545(11) 0.37085(16) 0.0383(4) Uani 1 1 d .
H5 H 1.1709 0.9712 0.3812 0.046 Uiso 1 1 calc R
C6 C 1.08360(9) 0.88951(9) 0.27337(13) 0.0233(3) Uani 1 1 d .
C7 C 1.10205(9) 0.94649(9) 0.17342(13) 0.0220(3) Uani 1 1 d .
N N 1.02246(7) 0.81103(7) 0.25846(10) 0.0191(3) Uani 1 1 d .
O1 O 0.94586(7) 0.60835(7) 0.34976(10) 0.0316(3) Uani 1 1 d .
O2 O 0.88091(6) 0.66328(6) 0.25450(10) 0.0275(3) Uani 1 1 d .
O3 O 1.14591(8) 1.02250(7) 0.19039(10) 0.0356(3) Uani 1 1 d .
O4 O 1.07271(6) 0.91094(6) 0.08041(9) 0.0245(3) Uani 1 1 d .
Ca Ca 0.926936(17) 0.781855(17) 0.09563(2) 0.01612(11) 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 0.0033 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'
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 126.99(14) . .
O1 C1 C2 117.33(13) . .
O2 C1 C2 115.68(12) . .
N C2 C3 122.70(14) . .
N C2 C1 114.56(12) . .
C3 C2 C1 122.75(13) . .
C2 C3 C4 118.39(15) . .
C5 C4 C3 119.14(16) . .
C4 C5 C6 118.64(16) . .
N C6 C5 122.24(14) . .
N C6 C7 115.32(13) . .
C5 C6 C7 122.29(14) . .
O3 C7 O4 126.93(14) . .
O3 C7 C6 117.05(14) . .
O4 C7 C6 115.99(13) . .
C2 N C6 118.63(13) . .
C2 N Ca 123.37(9) . .
C6 N Ca 117.58(9) . .
C1 O1 Ca 149.49(11) . 5_655
C1 O2 Ca 129.56(9) . 13_665
C1 O2 Ca 114.95(9) . .
Ca O2 Ca 114.15(4) 13_665 .
C7 O3 Ca 140.88(11) . 2_765
C7 O4 Ca 128.80(10) . 12_655
C7 O4 Ca 113.66(9) . .
Ca O4 Ca 115.76(4) 12_655 .
O3 Ca O1 171.16(5) 3_675 9_664
O3 Ca O2 87.63(4) 3_675 13_665
O1 Ca O2 100.11(4) 9_664 13_665
O3 Ca O4 90.10(4) 3_675 11_565
O1 Ca O4 94.27(4) 9_664 11_565
O2 Ca O4 89.10(4) 13_665 11_565
O3 Ca N 86.66(4) 3_675 .
O1 Ca N 85.27(4) 9_664 .
O2 Ca N 126.92(4) 13_665 .
O4 Ca N 143.57(4) 11_565 .
O3 Ca O4 92.11(4) 3_675 .
O1 Ca O4 81.05(4) 9_664 .
O2 Ca O4 169.66(4) 13_665 .
O4 Ca O4 80.56(4) 11_565 .
N Ca O4 63.35(4) . .
O3 Ca O2 94.31(4) 3_675 .
O1 Ca O2 85.08(4) 9_664 .
O2 Ca O2 65.85(4) 13_665 .
O4 Ca O2 154.30(4) 11_565 .
N Ca O2 62.07(4) . .
O4 Ca O2 124.46(3) . .
O3 Ca Ca 115.84(3) 3_675 12_655
O1 Ca Ca 60.02(3) 9_664 12_655
O2 Ca Ca 141.87(3) 13_665 12_655
O4 Ca Ca 62.88(3) 11_565 12_655
N Ca Ca 86.14(3) . 12_655
O4 Ca Ca 31.11(2) . 12_655
O2 Ca Ca 135.14(3) . 12_655
O3 Ca Ca 64.31(3) 3_675 11_565
O1 Ca Ca 122.43(3) 9_664 11_565
O2 Ca Ca 68.79(3) 13_665 11_565
O4 Ca Ca 33.13(2) 11_565 11_565
N Ca Ca 147.63(3) . 11_565
O4 Ca Ca 101.81(2) . 11_565
O2 Ca Ca 130.29(2) . 11_565
Ca Ca Ca 93.693(9) 12_655 11_565
O3 Ca Ca 91.38(3) 3_675 13_665
O1 Ca Ca 92.55(3) 9_664 13_665
O2 Ca Ca 35.08(3) 13_665 13_665
O4 Ca Ca 123.97(3) 11_565 13_665
N Ca Ca 92.39(3) . 13_665
O4 Ca Ca 155.21(3) . 13_665
O2 Ca Ca 30.77(2) . 13_665
Ca Ca Ca 152.559(10) 12_655 13_665
Ca Ca Ca 101.804(10) 11_565 13_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.2419(18) .
C1 O2 1.2525(18) .
C1 C2 1.511(2) .
C2 N 1.3329(19) .
C2 C3 1.380(2) .
C3 C4 1.383(2) .
C4 C5 1.380(3) .
C5 C6 1.385(2) .
C6 N 1.3331(18) .
C6 C7 1.511(2) .
C7 O3 1.2393(18) .
C7 O4 1.2630(18) .
N Ca 2.4932(12) .
O1 Ca 2.2865(10) 5_655
O2 Ca 2.3956(10) 13_665
O2 Ca 2.6917(11) .
O3 Ca 2.2739(11) 2_765
O4 Ca 2.4236(11) 12_655
O4 Ca 2.5632(10) .
Ca O3 2.2739(11) 3_675
Ca O1 2.2867(11) 9_664
Ca O2 2.3956(11) 13_665
Ca O4 2.4236(11) 11_565
Ca Ca 4.2241(4) 12_655
Ca Ca 4.2241(4) 11_565
Ca Ca 4.2732(6) 13_665
