#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:27:18 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179664 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/17/4511789.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_4511789
loop_
_publ_author_name
'White, Keith F.'
'Abrahams, Brendan F.'
'Maynard-Casely, Helen'
'Robson, Richard'
_publ_section_title
;
 Li+and Ca2+Derivatives of the Isonicotinate-N-oxide Ion Including Single
 Crystal-to-Single Crystal Transformations
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4602
_journal_paper_doi               10.1021/cg500710t
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C12 H12 Ca N2 O8'
_chemical_formula_weight         352.32
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 95.497(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.93380(10)
_cell_length_b                   9.83530(10)
_cell_length_c                   8.8614(2)
_cell_measurement_reflns_used    2273
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      75.3962
_cell_measurement_theta_min      4.4861
_cell_volume                     688.287(19)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.2273
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '/w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4146
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.989
_diffrn_reflns_theta_min         5.602
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       block
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1286
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0671P)²+0.3310P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1237
_reflns_number_total             1286
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg500710t_si_002.cif
_cod_data_source_block           RehydratedCa(inox)2
_cod_depositor_comments
'Adding full bibliography for 4511785--4511789.cif.'
_cod_database_code               4511789
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelxl_version_number           2014-1
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
H31 H 0.857(3) 0.522(3) 0.103(2) 0.039(8) Uiso 1 1 d D . .
H32 H 0.832(3) 0.577(3) -0.0461(16) 0.031(7) Uiso 1 1 d D . .
Ca1 Ca 0.5000 0.5000 0.0000 0.0087(2) Uani 1 2 d S . P
O1 O 0.52249(16) 0.36264(12) 0.20500(13) 0.0155(3) Uani 1 1 d . . .
O4 O 0.96610(15) 0.58064(12) 0.78288(13) 0.0158(3) Uani 1 1 d . . .
O3 O 0.79201(15) 0.56157(12) 0.03622(14) 0.0159(3) Uani 1 1 d D . .
O2 O 0.56456(16) 0.17552(12) 0.34382(13) 0.0156(3) Uani 1 1 d . . .
C5 C 0.8983(2) 0.37848(18) 0.65640(19) 0.0141(4) Uani 1 1 d . . .
H5 H 0.9735 0.3306 0.7275 0.017 Uiso 1 1 calc R U .
N1 N 0.88197(19) 0.51457(14) 0.66794(18) 0.0126(4) Uani 1 1 d . . .
C2 C 0.69775(19) 0.37772(17) 0.43578(18) 0.0115(4) Uani 1 1 d . . .
C1 C 0.5865(2) 0.29919(16) 0.31814(18) 0.0117(4) Uani 1 1 d . . .
C6 C 0.7808(2) 0.58564(17) 0.56399(18) 0.0134(4) Uani 1 1 d . . .
H6 H 0.7728 0.6817 0.5724 0.016 Uiso 1 1 calc R U .
C3 C 0.8061(2) 0.30908(17) 0.54174(19) 0.0139(4) Uani 1 1 d . . .
H3 H 0.8168 0.2131 0.5351 0.017 Uiso 1 1 calc R U .
C4 C 0.6894(2) 0.51891(18) 0.4463(2) 0.0131(4) Uani 1 1 d . . .
H4 H 0.6207 0.5692 0.3723 0.016 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 '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 O1 180.0 3_665 .
O1 Ca1 O2 88.28(4) 3_665 4_565
O1 Ca1 O2 91.72(4) . 4_565
O1 Ca1 O2 91.72(4) 3_665 2_655
O1 Ca1 O2 88.28(4) . 2_655
O2 Ca1 O2 180.00(4) 4_565 2_655
O1 Ca1 O3 87.55(4) 3_665 .
O1 Ca1 O3 92.45(4) . .
O2 Ca1 O3 90.12(4) 4_565 .
O2 Ca1 O3 89.88(4) 2_655 .
O1 Ca1 O3 92.45(4) 3_665 3_665
O1 Ca1 O3 87.55(4) . 3_665
O2 Ca1 O3 89.88(4) 4_565 3_665
O2 Ca1 O3 90.12(4) 2_655 3_665
O3 Ca1 O3 180.0 . 3_665
C1 O1 Ca1 160.27(12) . .
C1 O2 Ca1 151.72(11) . 2_645
N1 C5 C3 120.01(15) . .
O4 N1 C5 119.79(15) . .
O4 N1 C6 119.24(14) . .
C5 N1 C6 120.96(15) . .
C3 C2 C4 118.05(16) . .
C3 C2 C1 120.10(15) . .
C4 C2 C1 121.78(15) . .
O1 C1 O2 125.38(15) . .
O1 C1 C2 117.69(14) . .
O2 C1 C2 116.93(14) . .
N1 C6 C4 120.19(16) . .
C5 C3 C2 120.68(16) . .
C6 C4 C2 120.01(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.2572(12) 3_665
Ca1 O1 2.2572(12) .
Ca1 O2 2.3008(12) 4_565
Ca1 O2 2.3008(11) 2_655
Ca1 O3 2.3863(12) .
Ca1 O3 2.3863(12) 3_665
O1 C1 1.247(2) .
O4 N1 1.3322(19) .
O2 C1 1.253(2) .
O2 Ca1 2.3008(11) 2_645
C5 N1 1.350(2) .
C5 C3 1.375(2) .
N1 C6 1.356(2) .
C2 C3 1.386(2) .
C2 C4 1.394(3) .
C2 C1 1.512(2) .
C6 C4 1.378(2) .
