#------------------------------------------------------------------------------
#$Date: 2017-11-18 02:00:51 +0200 (Sat, 18 Nov 2017) $
#$Revision: 203308 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/42/4514294.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_4514294
loop_
_publ_author_name
'Rashchenko, Sergey V.'
'Bakakin, Vladimir V.'
'Shatskiy, Anton F.'
'Gavryushkin, Pavel N.'
'Seryotkin, Yurii V.'
'Litasov, Konstantin D.'
_publ_section_title
;
 Noncentrosymmetric Na2Ca4(CO3)5 Carbonate of “M13M23XY3Z”
 Structural Type and Affinity between Borate and Carbonate Structures for
 Design of New Optical Materials
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              6079
_journal_paper_doi               10.1021/acs.cgd.7b01161
_journal_volume                  17
_journal_year                    2017
_chemical_formula_sum            'C5 Ca4 Na2 O15'
_chemical_formula_weight         506.35
_chemical_name_systematic        'disodium tetracalcium pentacarbonate'
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_atom_sites_solution_hydrogens   .
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.37402(14)
_cell_length_b                   10.37402(14)
_cell_length_c                   6.25935(9)
_cell_measurement_reflns_used    15427
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4840
_cell_measurement_theta_min      3.9010
_cell_volume                     583.383(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            28295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.527
_diffrn_reflns_theta_min         2.267
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.035
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.883
_exptl_crystal_description       platelet
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 279 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         636
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0199
_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)+(0.0253P)²+0.3286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0505
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                625
_reflns_number_total             636
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Na2Ca4.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        583.383(17)
_cod_database_code               4514294
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.47699(5) 0.52301(5) 0.84198(18) 0.0142(2) Uani 0.6667 2 d S T P . .
Ca1 Ca 0.47699(5) 0.52301(5) 0.84198(18) 0.0142(2) Uani 0.3333 2 d S T P . .
Ca2 Ca 0.69199(7) 0.84599(4) 0.53142(13) 0.01567(16) Uani 1 2 d S T P . .
C1 C 1.000000 1.000000 0.3623(9) 0.0110(9) Uani 1 6 d S T P . .
O1 O 0.8579(3) 0.92895(13) 0.8661(4) 0.0209(5) Uani 1 2 d S T P . .
C2 C 0.6045(3) 0.80223(17) 0.0674(5) 0.0099(6) Uani 1 2 d S T P . .
O2 O 0.5511(3) 0.77555(14) 0.8792(4) 0.0163(5) Uani 1 2 d S T P . .
O3 O 0.7085(2) 1.07707(19) 0.6632(3) 0.0185(4) Uani 1 1 d . . . . .
C3 C 0.333333 0.666667 0.5079(9) 0.0117(10) Uani 1 6 d S T P . .
O4 O 0.40441(15) 0.59559(15) 0.5101(5) 0.0298(7) Uani 1 2 d S T P . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
O2 Ca1 O2 92.58(12) . 3_565
O2 Ca1 O3 155.01(9) . 3_565
O2 Ca1 O3 80.08(8) 3_565 3_565
O2 Ca1 O3 80.08(8) . 9_565
O2 Ca1 O3 155.01(9) 3_565 9_565
O3 Ca1 O3 96.52(10) 3_565 9_565
O2 Ca1 O4 124.69(7) . 4_665
O2 Ca1 O4 124.69(7) 3_565 4_665
O3 Ca1 O4 77.88(7) 3_565 4_665
O3 Ca1 O4 77.88(7) 9_565 4_665
O2 Ca1 O4 73.77(8) . .
O2 Ca1 O4 73.77(8) 3_565 .
O3 Ca1 O4 81.24(7) 3_565 .
O3 Ca1 O4 81.24(7) 9_565 .
O4 Ca1 O4 148.39(12) 4_665 .
O2 Ca1 O3 51.73(7) . 6_655
O2 Ca1 O3 109.20(9) 3_565 6_655
O3 Ca1 O3 153.13(7) 3_565 6_655
O3 Ca1 O3 85.02(6) 9_565 6_655
O4 Ca1 O3 76.23(7) 4_665 6_655
O4 Ca1 O3 125.32(6) . 6_655
O2 Ca1 O3 109.20(9) . 12_655
O2 Ca1 O3 51.73(7) 3_565 12_655
O3 Ca1 O3 85.02(6) 3_565 12_655
O3 Ca1 O3 153.13(7) 9_565 12_655
O4 Ca1 O3 76.23(7) 4_665 12_655
O4 Ca1 O3 125.32(6) . 12_655
O3 Ca1 O3 81.97(8) 6_655 12_655
O2 Ca1 C2 25.64(8) . 1_556
O2 Ca1 C2 99.04(9) 3_565 1_556
O3 Ca1 C2 178.73(9) 3_565 1_556
O3 Ca1 C2 84.66(7) 9_565 1_556
O4 Ca1 C2 101.97(7) 4_665 1_556
O4 Ca1 C2 99.40(7) . 1_556
O3 Ca1 C2 26.41(6) 6_655 1_556
O3 Ca1 C2 93.72(8) 12_655 1_556
O2 Ca1 C2 99.04(9) . 3_566
O2 Ca1 C2 25.64(8) 3_565 3_566
O3 Ca1 C2 84.66(7) 3_565 3_566
O3 Ca1 C2 178.73(9) 9_565 3_566
O4 Ca1 C2 101.97(7) 4_665 3_566
O4 Ca1 C2 99.40(7) . 3_566
O3 Ca1 C2 93.72(8) 6_655 3_566
O3 Ca1 C2 26.41(6) 12_655 3_566
C2 Ca1 C2 94.15(12) 1_556 3_566
O2 Ca1 Na1 94.51(7) . 4_665
O2 Ca1 Na1 94.51(7) 3_565 4_665
O3 Ca1 Na1 109.77(6) 3_565 4_665
O3 Ca1 Na1 109.77(6) 9_565 4_665
O4 Ca1 Na1 48.92(8) 4_665 4_665
O4 Ca1 Na1 162.68(9) . 4_665
O3 Ca1 Na1 45.86(4) 6_655 4_665
O3 Ca1 Na1 45.86(4) 12_655 4_665
C2 Ca1 Na1 69.35(5) 1_556 4_665
C2 Ca1 Na1 69.35(5) 3_566 4_665
O2 Ca1 Na1 105.71(7) . 4_664
O2 Ca1 Na1 105.71(7) 3_565 4_664
O3 Ca1 Na1 54.74(6) 3_565 4_664
O3 Ca1 Na1 54.74(6) 9_565 4_664
O4 Ca1 Na1 101.48(9) 4_665 4_664
O4 Ca1 Na1 46.92(7) . 4_664
O3 Ca1 Na1 138.54(4) 6_655 4_664
O3 Ca1 Na1 138.54(4) 12_655 4_664
C2 Ca1 Na1 126.47(6) 1_556 4_664
C2 Ca1 Na1 126.47(6) 3_566 4_664
Na1 Ca1 Na1 150.40(7) 4_665 4_664
O3 Ca2 O3 140.14(9) . 9_565
O3 Ca2 O2 74.95(5) . .
O3 Ca2 O2 74.95(5) 9_565 .
O3 Ca2 O1 72.04(5) . .
O3 Ca2 O1 72.04(5) 9_565 .
O2 Ca2 O1 65.61(8) . .
O3 Ca2 O1 71.68(7) . 5_564
O3 Ca2 O1 118.78(7) 9_565 5_564
O2 Ca2 O1 138.77(7) . 5_564
O1 Ca2 O1 81.39(6) . 5_564
O3 Ca2 O1 118.78(7) . 6_654
O3 Ca2 O1 71.68(7) 9_565 6_654
O2 Ca2 O1 138.77(7) . 6_654
O1 Ca2 O1 81.39(6) . 6_654
O1 Ca2 O1 50.07(10) 5_564 6_654
O3 Ca2 O3 135.05(7) . 6_654
O3 Ca2 O3 84.75(5) 9_565 6_654
O2 Ca2 O3 131.08(6) . 6_654
O1 Ca2 O3 146.96(5) . 6_654
O1 Ca2 O3 90.01(7) 5_564 6_654
O1 Ca2 O3 68.93(7) 6_654 6_654
O3 Ca2 O3 84.75(5) . 11_674
O3 Ca2 O3 135.05(7) 9_565 11_674
O2 Ca2 O3 131.08(6) . 11_674
O1 Ca2 O3 146.96(5) . 11_674
O1 Ca2 O3 68.93(7) 5_564 11_674
O1 Ca2 O3 90.01(7) 6_654 11_674
O3 Ca2 O3 50.31(8) 6_654 11_674
O3 Ca2 O4 116.17(8) . .
O3 Ca2 O4 72.66(7) 9_565 .
O2 Ca2 O4 65.13(8) . .
O1 Ca2 O4 124.82(9) . .
O1 Ca2 O4 153.61(9) 5_564 .
O1 Ca2 O4 124.27(8) 6_654 .
O3 Ca2 O4 66.44(8) 6_654 .
O3 Ca2 O4 86.24(7) 11_674 .
O3 Ca2 O4 72.66(7) . 2_665
O3 Ca2 O4 116.17(8) 9_565 2_665
O2 Ca2 O4 65.13(8) . 2_665
O1 Ca2 O4 124.82(9) . 2_665
O1 Ca2 O4 124.27(8) 5_564 2_665
O1 Ca2 O4 153.61(9) 6_654 2_665
O3 Ca2 O4 86.24(7) 6_654 2_665
O3 Ca2 O4 66.44(8) 11_674 2_665
O4 Ca2 O4 46.30(11) . 2_665
O3 Ca2 C1 93.63(6) . .
O3 Ca2 C1 93.63(6) 9_565 .
O2 Ca2 C1 141.11(12) . .
O1 Ca2 C1 75.50(12) . .
O1 Ca2 C1 25.50(6) 5_564 .
O1 Ca2 C1 25.50(6) 6_654 .
O3 Ca2 C1 83.07(10) 6_654 .
O3 Ca2 C1 83.07(10) 11_674 .
O4 Ca2 C1 147.21(9) . .
O4 Ca2 C1 147.21(9) 2_665 .
O3 Ca2 C2 109.85(5) . .
O3 Ca2 C2 109.85(5) 9_565 .
O2 Ca2 C2 134.67(8) . .
O1 Ca2 C2 159.71(8) . .
O1 Ca2 C2 80.25(8) 5_564 .
O1 Ca2 C2 80.25(8) 6_654 .
O3 Ca2 C2 25.22(4) 6_654 .
O3 Ca2 C2 25.22(4) 11_674 .
O4 Ca2 C2 73.39(8) . .
O4 Ca2 C2 73.39(8) 2_665 .
C1 Ca2 C2 84.21(11) . .
O1 C1 O1 119.966(19) 4_774 6_654
O1 C1 O1 119.97(2) 4_774 5_564
O1 C1 O1 119.97(2) 6_654 5_564
O1 C1 Ca2 158.0(4) 4_774 .
O1 C1 Ca2 61.73(10) 6_654 .
O1 C1 Ca2 61.73(10) 5_564 .
O1 C1 Ca2 61.73(10) 4_774 3_675
O1 C1 Ca2 158.0(4) 6_654 3_675
O1 C1 Ca2 61.73(10) 5_564 3_675
Ca2 C1 Ca2 107.97(10) . 3_675
O1 C1 Ca2 61.73(10) 4_774 2_765
O1 C1 Ca2 61.74(10) 6_654 2_765
O1 C1 Ca2 158.0(4) 5_564 2_765
Ca2 C1 Ca2 107.97(10) . 2_765
Ca2 C1 Ca2 107.97(10) 3_675 2_765
C1 O1 Ca2 124.4(3) 4_775 .
C1 O1 Ca2 92.77(12) 4_775 6_655
Ca2 O1 Ca2 107.40(6) . 6_655
C1 O1 Ca2 92.77(12) 4_775 5_565
Ca2 O1 Ca2 107.40(6) . 5_565
Ca2 O1 Ca2 133.06(12) 6_655 5_565
O2 C2 O3 120.18(15) 1_554 6_654
O2 C2 O3 120.18(15) 1_554 11_674
O3 C2 O3 119.6(3) 6_654 11_674
O2 C2 Na1 52.88(6) 1_554 2_664
O3 C2 Na1 166.9(2) 6_654 2_664
O3 C2 Na1 68.43(12) 11_674 2_664
O2 C2 Na1 52.88(6) 1_554 1_554
O3 C2 Na1 68.44(12) 6_654 1_554
O3 C2 Na1 166.9(2) 11_674 1_554
Na1 C2 Na1 101.78(10) 2_664 1_554
O2 C2 Ca2 173.0(2) 1_554 .
O3 C2 Ca2 60.06(15) 6_654 .
O3 C2 Ca2 60.06(15) 11_674 .
Na1 C2 Ca2 125.22(6) 2_664 .
Na1 C2 Ca2 125.22(6) 1_554 .
C2 O2 Na1 101.48(8) 1_556 2_665
C2 O2 Ca1 101.48(8) 1_556 .
Na1 O2 Ca1 144.97(12) 2_665 .
C2 O2 Ca2 127.7(2) 1_556 .
Na1 O2 Ca2 93.26(7) 2_665 .
Ca1 O2 Ca2 93.26(7) . .
C2 O3 Na1 144.66(18) 5_565 2_665
C2 O3 Ca2 116.31(17) 5_565 .
Na1 O3 Ca2 94.32(7) 2_665 .
C2 O3 Ca2 94.72(15) 5_565 5_565
Na1 O3 Ca2 89.96(7) 2_665 5_565
Ca2 O3 Ca2 110.78(7) . 5_565
C2 O3 Na1 85.15(15) 5_565 5_564
Na1 O3 Na1 79.40(6) 2_665 5_564
Ca2 O3 Na1 86.30(6) . 5_564
Ca2 O3 Na1 160.66(8) 5_565 5_564
O4 C3 O4 119.989(12) 3_565 2_665
O4 C3 O4 119.989(13) 3_565 .
O4 C3 O4 119.989(14) 2_665 .
O4 C3 Ca2 60.004(14) 3_565 2_665
O4 C3 Ca2 60.004(14) 2_665 2_665
O4 C3 Ca2 176.8(4) . 2_665
O4 C3 Ca2 60.004(14) 3_565 3_565
O4 C3 Ca2 176.8(4) 2_665 3_565
O4 C3 Ca2 60.004(14) . 3_565
Ca2 C3 Ca2 119.794(17) 2_665 3_565
O4 C3 Ca2 176.8(4) 3_565 .
O4 C3 Ca2 60.004(14) 2_665 .
O4 C3 Ca2 60.004(14) . .
Ca2 C3 Ca2 119.794(17) 2_665 .
Ca2 C3 Ca2 119.794(17) 3_565 .
C3 O4 Na1 153.1(4) . 4_664
C3 O4 Ca1 122.7(3) . .
Na1 O4 Ca1 84.16(9) 4_664 .
C3 O4 Ca2 96.84(6) . 3_565
Na1 O4 Ca2 85.10(6) 4_664 3_565
Ca1 O4 Ca2 84.07(6) . 3_565
C3 O4 Ca2 96.85(6) . .
Na1 O4 Ca2 85.10(6) 4_664 .
Ca1 O4 Ca2 84.07(6) . .
Ca2 O4 Ca2 165.31(11) 3_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O2 2.3440(10) .
Ca1 O2 2.3440(10) 3_565
Ca1 O3 2.3635(19) 3_565
Ca1 O3 2.3635(19) 9_565
Ca1 O4 2.377(3) 4_665
Ca1 O4 2.453(3) .
Ca1 O3 2.689(2) 6_655
Ca1 O3 2.689(2) 12_655
Ca1 C2 2.881(2) 1_556
Ca1 C2 2.881(2) 3_566
Ca2 O3 2.4586(18) .
Ca2 O3 2.4586(18) 9_565
Ca2 O2 2.518(3) .
Ca2 O1 2.571(3) .
Ca2 O1 2.6126(13) 5_564
Ca2 O1 2.6126(13) 6_654
Ca2 O3 2.616(2) 6_654
Ca2 O3 2.616(2) 11_674
Ca2 O4 2.8136(7) .
Ca2 O4 2.8136(7) 2_665
Ca2 C1 2.963(2) .
Ca2 C2 3.009(3) .
C1 O1 1.277(2) 4_774
C1 O1 1.277(2) 6_654
C1 O1 1.277(2) 5_564
C2 O2 1.272(4) 1_554
C2 O3 1.286(2) 6_654
C2 O3 1.286(2) 11_674
C3 O4 1.277(3) 3_565
C3 O4 1.277(3) 2_665
C3 O4 1.277(3) .
