#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:33:26 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179535 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/04/4500463.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_4500463
loop_
_publ_author_name
'Kim, Min Kyung'
'Bae, Kyung-Lyul'
'Ok, Kang Min'
_publ_section_title
;
 From Pincers to Steps: Synthesis, Structure, Characterization, and
 Transformation of a New Helical Calcium−Organic Framework,
 Ca[NC5H3(CO2)2](H2O)1.5
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              930
_journal_paper_doi               10.1021/cg101558e
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C14 H12 Ca2 N2 O11'
_chemical_formula_weight         464.4
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 92.64(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.658(3)
_cell_length_b                   9.837(2)
_cell_length_c                   13.586(3)
_cell_measurement_temperature    200.0(2)
_cell_volume                     1823.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200.0(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.1077
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6505
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.69
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS(Blessing, 1995) 
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.763
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0390P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                1292
_reflns_number_total             2191
_reflns_threshold_expression     >2Ĭ)
_cod_data_source_file            cg101558e_si_002.cif
_cod_data_source_block           Ca-org1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1823.3(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4500463
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ca1 Ca 0.04881(6) 0.01088(8) 0.87124(5) 0.0194(2) Uani 1 1 d .
O1 O 0.1775(2) -0.1153(3) 0.9380(2) 0.0337(8) Uani 1 1 d .
H1' H 0.1571 -0.1688 0.9786 0.051 Uiso 1 1 calc R
O2 O 0 -0.1605(4) 0.75 0.0238(10) Uani 1 2 d S
O3 O 0.0439(2) 0.1288(3) 1.02558(18) 0.0228(7) Uani 1 1 d .
O4 O 0.0913(3) 0.3065(3) 1.11956(19) 0.0431(9) Uani 1 1 d .
O5 O 0.09760(19) 0.0927(3) 0.70781(18) 0.0222(6) Uani 1 1 d .
O6 O 0.1567(2) 0.2565(3) 0.61306(18) 0.0294(7) Uani 1 1 d .
N1 N 0.1097(2) 0.2469(3) 0.8658(2) 0.0230(8) Uani 1 1 d .
C2 C 0.1060(3) 0.3239(4) 0.9477(3) 0.0249(10) Uani 1 1 d .
C3 C 0.1232(4) 0.4629(5) 0.9469(3) 0.0338(12) Uani 1 1 d .
C4 C 0.1439(4) 0.5236(5) 0.8578(3) 0.0354(12) Uani 1 1 d .
C5 C 0.1491(3) 0.4450(4) 0.7736(3) 0.0324(11) Uani 1 1 d .
C6 C 0.1316(3) 0.3073(4) 0.7812(3) 0.0223(9) Uani 1 1 d .
C7 C 0.0795(3) 0.2478(4) 1.0387(3) 0.0250(10) Uani 1 1 d .
C8 C 0.1296(3) 0.2125(4) 0.6934(3) 0.0208(9) Uani 1 1 d .
H1 H 0.237 -0.150 0.919 0.10 Uiso 1 1 d .
H2 H -0.035 -0.212 0.788 0.049 Uiso 1 1 d .
H3 H 0.120 0.516 1.006 0.045 Uiso 1 1 d .
H4 H 0.159 0.621 0.854 0.046 Uiso 1 1 d .
H5 H 0.165 0.490 0.708 0.030 Uiso 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 0 '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 0.006 '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 Ca1 O5 167.25(11) . 2_556
O1 Ca1 O3 82.72(11) . 5_557
O5 Ca1 O3 90.14(10) 2_556 5_557
O1 Ca1 O3 88.16(10) . .
O5 Ca1 O3 100.07(9) 2_556 .
O3 Ca1 O3 74.11(10) 5_557 .
O1 Ca1 O2 94.23(10) . .
O5 Ca1 O2 74.24(9) 2_556 .
O3 Ca1 O2 82.02(8) 5_557 .
O3 Ca1 O2 155.53(8) . .
O1 Ca1 N1 105.46(12) . .
O5 Ca1 N1 86.87(10) 2_556 .
O3 Ca1 N1 138.81(10) 5_557 .
O3 Ca1 N1 66.06(9) . .
O2 Ca1 N1 135.66(10) . .
O1 Ca1 O5 107.20(10) . .
O5 Ca1 O5 74.92(11) 2_556 .
O3 Ca1 O5 152.85(9) 5_557 .
O3 Ca1 O5 130.13(9) . .
O2 Ca1 O5 72.24(8) . .
N1 Ca1 O5 64.14(9) . .
O1 Ca1 C8 171.78(10) . 2_556
O5 Ca1 C8 19.51(9) 2_556 2_556
O3 Ca1 C8 95.75(10) 5_557 2_556
O3 Ca1 C8 83.66(10) . 2_556
O2 Ca1 C8 93.54(9) . 2_556
N1 Ca1 C8 70.44(10) . 2_556
O5 Ca1 C8 77.76(9) . 2_556
O1 Ca1 Ca1 128.47(8) . 2_556
O5 Ca1 Ca1 45.16(7) 2_556 2_556
O3 Ca1 Ca1 111.49(7) 5_557 2_556
O3 Ca1 Ca1 142.96(7) . 2_556
O2 Ca1 Ca1 43.96(7) . 2_556
N1 Ca1 Ca1 94.95(7) . 2_556
O5 Ca1 Ca1 42.56(6) . 2_556
C8 Ca1 Ca1 59.60(7) 2_556 2_556
O1 Ca1 Ca1 84.31(8) . 5_557
O5 Ca1 Ca1 96.42(7) 2_556 5_557
O3 Ca1 Ca1 37.33(6) 5_557 5_557
O3 Ca1 Ca1 36.79(6) . 5_557
O2 Ca1 Ca1 119.17(6) . 5_557
N1 Ca1 Ca1 102.28(8) . 5_557
O5 Ca1 Ca1 163.82(7) . 5_557
C8 Ca1 Ca1 89.59(7) 2_556 5_557
Ca1 Ca1 Ca1 137.00(5) 2_556 5_557
Ca1 O2 Ca1 92.07(14) . 2_556
C7 O3 Ca1 131.3(2) . 5_557
C7 O3 Ca1 122.6(2) . .
Ca1 O3 Ca1 105.89(10) 5_557 .
C8 O5 Ca1 122.2(2) . 2_556
C8 O5 Ca1 123.0(2) . .
Ca1 O5 Ca1 92.28(10) 2_556 .
C6 N1 C2 118.5(3) . .
C6 N1 Ca1 122.1(2) . .
C2 N1 Ca1 118.6(2) . .
N1 C2 C3 122.3(4) . .
N1 C2 C7 114.7(3) . .
C3 C2 C7 123.0(4) . .
C2 C3 C4 118.2(4) . .
C5 C4 C3 119.9(4) . .
C6 C5 C4 118.1(4) . .
N1 C6 C5 123.0(4) . .
N1 C6 C8 114.0(3) . .
C5 C6 C8 122.9(4) . .
O4 C7 O3 125.6(4) . .
O4 C7 C2 117.9(4) . .
O3 C7 C2 116.6(3) . .
O6 C8 O5 125.0(4) . .
O6 C8 C6 118.7(4) . .
O5 C8 C6 116.3(3) . .
O6 C8 Ca1 103.0(2) . 2_556
O5 C8 Ca1 38.30(17) . 2_556
C6 C8 Ca1 125.4(3) . 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.303(3) .
Ca1 O5 2.367(3) 2_556
Ca1 O3 2.370(3) 5_557
Ca1 O3 2.400(3) .
Ca1 O2 2.429(3) .
Ca1 N1 2.468(3) .
Ca1 O5 2.481(3) .
Ca1 C8 3.232(4) 2_556
Ca1 Ca1 3.4965(17) 2_556
Ca1 Ca1 3.8071(18) 5_557
O2 Ca1 2.429(3) 2_556
O3 C7 1.276(5) .
O3 Ca1 2.370(3) 5_557
O4 C7 1.246(4) .
O5 C8 1.276(5) .
O5 Ca1 2.367(3) 2_556
O6 C8 1.247(4) .
N1 C6 1.341(5) .
N1 C2 1.349(5) .
C2 C3 1.387(6) .
C2 C7 1.503(5) .
C3 C4 1.390(6) .
C4 C5 1.386(6) .
C5 C6 1.380(6) .
C6 C8 1.513(5) .
C8 Ca1 3.232(4) 2_556
