#------------------------------------------------------------------------------
#$Date: 2026-04-23 01:18:41 +0200 (Thu, 23 Apr 2026) $
#$Revision: 305598 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/72/09/7720909.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_7720909
loop_
_publ_author_name
'Elkik, Hussin'
'Iqbal, Muhammad Mujahid'
'Munawar, Aqsa'
'Yang, Zhihua'
'Zhang, Fangfang'
'Pan, Shilie'
_publ_section_title
;
 Synthesis and characterization of hydrated alkali metal calcium nitrates
 ACa(NO₃)₃·2H₂O (A = NH₄,
 Rb, Cs) as short ultraviolet birefringent materials.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d6dt00380j
_journal_year                    2026
_chemical_formula_moiety         'Ca H4 N3 O11, H4 N'
_chemical_formula_sum            'Ca H8 N4 O11'
_chemical_formula_weight         280.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2026-03-13
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2026.02.28 svn.rb976bf26 for OlexSys, GUI svn.r7508)
;
_audit_update_record
;
2026-03-23 deposited with the CCDC.	2026-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                99.129(4)
_cell_angle_beta                 91.341(4)
_cell_angle_gamma                91.711(4)
_cell_formula_units_Z            2
_cell_length_a                   6.4805(6)
_cell_length_b                   7.4530(7)
_cell_length_c                   10.4970(10)
_cell_measurement_reflns_used    6496
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.15
_cell_volume                     500.15(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13413
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         1.966
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0637 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.9567.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_description       block
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.037(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0292
_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)+(0.0345P)²+0.1810P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2143
_reflns_number_total             2288
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00380j2.cif
_cod_data_source_block           hu52-collect
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7720909
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.922
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O4(H4a,H4b)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Ca1 Ca 0.75956(4) 0.42623(4) 0.25019(3) 0.02511(12) Uani 1 1 d . . . . .
O2 O 0.58446(17) 0.70283(16) 0.36666(12) 0.0383(3) Uani 1 1 d . . . . .
O3 O 0.91553(16) 0.72008(16) 0.36749(12) 0.0375(3) Uani 1 1 d . . . . .
O4 O 0.74528(18) 0.35789(19) 0.46278(11) 0.0414(3) Uani 1 1 d . . . . .
H4A H 0.848311 0.288412 0.477644 0.062 Uiso 1 1 d R U . . .
H4B H 0.634071 0.289534 0.470294 0.062 Uiso 1 1 d R U . . .
O9 O 0.7663(2) 0.21960(15) 0.04173(12) 0.0439(3) Uani 1 1 d . . . . .
O7 O 0.08880(18) 0.29047(19) 0.29481(15) 0.0491(3) Uani 1 1 d . . . . .
O10 O 0.7328(2) 0.05759(19) 0.19178(12) 0.0481(3) Uani 1 1 d . . . . .
N1 N 0.74922(19) 0.79235(17) 0.40571(12) 0.0312(3) Uani 1 1 d . . . . .
O5 O 0.7071(3) 0.5956(2) 0.08223(14) 0.0600(5) Uani 1 1 d . . . . .
N3 N 0.7489(2) 0.06575(17) 0.07520(13) 0.0339(3) Uani 1 1 d . . . . .
O6 O 0.40801(17) 0.3192(2) 0.25892(16) 0.0562(4) Uani 1 1 d . . . . .
O11 O 0.7467(3) -0.07151(17) -0.00749(14) 0.0608(4) Uani 1 1 d . . . . .
N2 N 0.2309(2) 0.37246(18) 0.24808(13) 0.0328(3) Uani 1 1 d . . . . .
O1 O 0.7468(3) 0.93789(19) 0.47485(15) 0.0577(4) Uani 1 1 d . . . . .
N4 N 0.2593(3) 0.9095(2) 0.25021(17) 0.0427(4) Uani 1 1 d . . . . .
O8 O 0.1848(3) 0.4992(2) 0.19204(15) 0.0644(4) Uani 1 1 d . . . . .
H4C H 0.365(6) 0.867(5) 0.274(4) 0.113(13) Uiso 1 1 d . . . . .
H4D H 0.248(5) 0.888(5) 0.176(4) 0.105(12) Uiso 1 1 d . . . . .
H4E H 0.139(6) 0.870(5) 0.284(4) 0.116(13) Uiso 1 1 d . . . . .
H4F H 0.274(6) 1.018(6) 0.272(4) 0.129(15) Uiso 1 1 d . . . . .
H5A H 0.731(5) 0.704(5) 0.074(3) 0.090(10) Uiso 1 1 d . . . . .
H5B H 0.712(5) 0.538(5) 0.009(3) 0.098(11) 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
Ca Ca 0.2262 0.3064 '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'
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
_geom_angle_publ_flag
O2 Ca1 O10 143.97(4) . . ?
O2 Ca1 N1 25.24(4) . . ?
O2 Ca1 N3 151.87(4) . . ?
O2 Ca1 N2 125.21(4) . 1_655 ?
O2 Ca1 O8 113.33(4) . 1_655 ?
O3 Ca1 O2 50.33(4) . . ?
O3 Ca1 O10 153.22(4) . . ?
O3 Ca1 N1 25.12(3) . . ?
O3 Ca1 N3 156.83(4) . . ?
O3 Ca1 N2 75.11(4) . 1_655 ?
O3 Ca1 O8 64.95(4) . 1_655 ?
O4 Ca1 O2 78.46(4) . . ?
O4 Ca1 O3 81.93(4) . . ?
O4 Ca1 O9 129.78(5) . . ?
O4 Ca1 O7 73.23(4) . 1_655 ?
O4 Ca1 O10 81.36(4) . . ?
O4 Ca1 N1 78.13(4) . . ?
O4 Ca1 N3 105.74(4) . . ?
O4 Ca1 O6 77.88(5) . . ?
O4 Ca1 N2 90.80(4) . 1_655 ?
O4 Ca1 O8 109.07(4) . 1_655 ?
O9 Ca1 O2 142.92(4) . . ?
O9 Ca1 O3 141.80(4) . . ?
O9 Ca1 O10 48.49(4) . . ?
O9 Ca1 N1 152.06(4) . . ?
O9 Ca1 N3 24.07(4) . . ?
O9 Ca1 N2 82.85(4) . 1_655 ?
O9 Ca1 O8 82.55(5) . 1_655 ?
O7 Ca1 O2 131.23(5) 1_655 . ?
O7 Ca1 O3 86.55(4) 1_655 . ?
O7 Ca1 O9 84.35(5) 1_655 . ?
O7 Ca1 O10 68.64(5) 1_655 . ?
O7 Ca1 N1 108.80(4) 1_655 . ?
O7 Ca1 N3 75.25(4) 1_655 . ?
O7 Ca1 N2 22.32(4) 1_655 1_655 ?
O7 Ca1 O8 45.73(4) 1_655 1_655 ?
O10 Ca1 N1 159.07(4) . . ?
O10 Ca1 N3 24.42(4) . . ?
O10 Ca1 N2 84.35(4) . 1_655 ?
O10 Ca1 O8 101.34(4) . 1_655 ?
N1 Ca1 N3 175.23(4) . . ?
N1 Ca1 N2 100.01(4) . 1_655 ?
O5 Ca1 O2 78.48(5) . . ?
O5 Ca1 O3 83.65(5) . . ?
O5 Ca1 O4 156.94(6) . . ?
O5 Ca1 O9 71.16(5) . . ?
O5 Ca1 O7 123.74(6) . 1_655 ?
O5 Ca1 O10 118.09(5) . . ?
O5 Ca1 N1 81.16(5) . . ?
O5 Ca1 N3 94.51(5) . . ?
O5 Ca1 O6 96.63(6) . . ?
O5 Ca1 N2 102.77(6) . 1_655 ?
O5 Ca1 O8 80.59(6) . 1_655 ?
N3 Ca1 N2 82.85(4) . 1_655 ?
O6 Ca1 O2 77.11(4) . . ?
O6 Ca1 O3 126.46(4) . . ?
O6 Ca1 O9 85.61(5) . . ?
O6 Ca1 O7 131.89(5) . 1_655 ?
O6 Ca1 O10 69.63(5) . . ?
O6 Ca1 N1 101.70(4) . . ?
O6 Ca1 N3 76.70(4) . . ?
O6 Ca1 N2 152.78(4) . 1_655 ?
O6 Ca1 O8 168.11(5) . 1_655 ?
O8 Ca1 N1 89.35(4) 1_655 . ?
O8 Ca1 N3 91.93(4) 1_655 . ?
O8 Ca1 N2 23.41(4) 1_655 1_655 ?
N1 O2 Ca1 96.05(8) . . ?
N1 O3 Ca1 97.53(8) . . ?
Ca1 O4 H4A 110.1 . . ?
Ca1 O4 H4B 110.0 . . ?
H4A O4 H4B 103.8 . . ?
N3 O9 Ca1 102.49(9) . . ?
N2 O7 Ca1 109.04(10) . 1_455 ?
N3 O10 Ca1 90.73(9) . . ?
O2 N1 Ca1 58.71(7) . . ?
O3 N1 Ca1 57.35(7) . . ?
O3 N1 O2 115.92(12) . . ?
O1 N1 Ca1 176.62(12) . . ?
O1 N1 O2 121.80(14) . . ?
O1 N1 O3 122.28(14) . . ?
Ca1 O5 H5A 134(2) . . ?
Ca1 O5 H5B 116(3) . . ?
H5A O5 H5B 105(3) . . ?
O9 N3 Ca1 53.44(8) . . ?
O10 N3 Ca1 64.85(9) . . ?
O10 N3 O9 118.28(14) . . ?
O11 N3 Ca1 173.03(11) . . ?
O11 N3 O9 119.59(14) . . ?
O11 N3 O10 122.13(14) . . ?
N2 O6 Ca1 139.83(12) . . ?
O7 N2 Ca1 48.63(8) . 1_455 ?
O6 N2 Ca1 166.44(12) . 1_455 ?
O6 N2 O7 117.87(15) . . ?
O8 N2 Ca1 69.05(11) . 1_455 ?
O8 N2 O7 117.68(15) . . ?
O8 N2 O6 124.44(17) . . ?
H4C N4 H4D 110(4) . . ?
H4C N4 H4E 116(3) . . ?
H4C N4 H4F 105(4) . . ?
H4D N4 H4E 107(3) . . ?
H4D N4 H4F 109(4) . . ?
H4E N4 H4F 109(3) . . ?
N2 O8 Ca1 87.55(11) . 1_455 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.5372(12) . ?
Ca1 O3 2.5076(12) . ?
Ca1 O4 2.3697(12) . ?
Ca1 O9 2.4699(13) . ?
Ca1 O7 2.4552(13) 1_655 ?
Ca1 O10 2.7178(15) . ?
Ca1 N1 2.9526(13) . ?
Ca1 O5 2.3497(13) . ?
Ca1 N3 3.0023(13) . ?
Ca1 O6 2.4000(12) . ?
Ca1 N2 3.0925(13) 1_655 ?
Ca1 O8 2.8906(19) 1_655 ?
O2 N1 1.2662(17) . ?
O3 N1 1.2645(17) . ?
O4 H4A 0.8830 . ?
O4 H4B 0.8824 . ?
O9 N3 1.2542(18) . ?
O7 N2 1.2427(18) . ?
O10 N3 1.2415(18) . ?
N1 O1 1.2064(18) . ?
O5 H5A 0.83(3) . ?
O5 H5B 0.82(4) . ?
N3 O11 1.2316(18) . ?
O6 N2 1.2345(18) . ?
N2 O8 1.230(2) . ?
N4 H4C 0.81(4) . ?
N4 H4D 0.77(4) . ?
N4 H4E 0.92(4) . ?
N4 H4F 0.81(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O4 H4A O3 0.88 2.22 2.9266(16) 137.3 2_766 yes
O4 H4A O7 0.88 2.50 2.8787(17) 106.4 1_655 yes
O4 H4A O1 0.88 2.67 3.153(2) 115.5 1_545 yes
O4 H4B O2 0.88 2.24 2.8904(16) 130.1 2_666 yes
O4 H4B O6 0.88 2.67 2.9979(19) 103.1 . yes
N4 H4C O2 0.81(4) 2.21(4) 2.997(2) 163(4) . yes
N4 H4D O9 0.77(4) 2.30(4) 3.062(2) 171(4) 2_665 yes
N4 H4D O11 0.77(4) 2.40(4) 2.987(2) 134(4) 2_665 yes
N4 H4E O3 0.92(4) 2.10(4) 2.994(2) 164(3) 1_455 yes
N4 H4E O8 0.92(4) 2.81(4) 3.044(2) 96(3) . yes
N4 H4F O7 0.81(4) 2.37(4) 3.048(2) 142(4) 1_565 yes
N4 H4F O6 0.81(4) 2.41(5) 3.161(2) 155(4) 1_565 yes
N4 H4F O1 0.81(4) 2.63(4) 2.931(2) 104(3) 2_676 yes
O5 H5A O11 0.83(3) 2.00(3) 2.7970(19) 159(3) 1_565 yes
O5 H5B O9 0.82(4) 2.49(4) 2.8061(19) 104(3) . yes
O5 H5B O8 0.82(4) 2.20(4) 2.959(2) 153(3) 2_665 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O2 N1 O3 4.12(13) . . . . ?
Ca1 O2 N1 O1 -176.08(14) . . . . ?
Ca1 O3 N1 O2 -4.18(13) . . . . ?
Ca1 O3 N1 O1 176.02(14) . . . . ?
Ca1 O9 N3 O10 0.53(17) . . . . ?
Ca1 O9 N3 O11 179.97(14) . . . . ?
Ca1 O7 N2 O6 -178.36(12) 1_455 . . . ?
Ca1 O7 N2 O8 0.32(17) 1_455 . . . ?
Ca1 O10 N3 O9 -0.47(15) . . . . ?
Ca1 O10 N3 O11 -179.90(16) . . . . ?
Ca1 O6 N2 Ca1 -165.5(3) . . . 1_455 ?
Ca1 O6 N2 O7 -160.21(15) . . . . ?
Ca1 O6 N2 O8 21.2(3) . . . . ?
O7 N2 O8 Ca1 -0.26(14) . . . 1_455 ?
O6 N2 O8 Ca1 178.32(15) . . . 1_455 ?
