#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:22:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229563 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/49/7044902.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_7044902
loop_
_publ_author_name
'Nimax, Patrick R.'
'Sünkel, Karlheinz'
_publ_section_title
;
 Structural diversity in the alkaline earth metal compounds of tetra and
 pentacyanocyclopentadienide.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              409
_journal_page_last               417
_journal_paper_doi               10.1039/c7dt03862c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C10 H10 Ca N5 O5, C10 N5, H2 O'
_chemical_formula_sum            'C20 H12 Ca N10 O6'
_chemical_formula_weight         528.48
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2017-08-04T08:52:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-08-17 deposited with the CCDC.
2017-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0319(5)
_cell_length_b                   12.4908(5)
_cell_length_c                   17.7452(8)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.3843
_cell_measurement_theta_min      2.4632
_cell_volume                     2445.24(18)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 Quest'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39685
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         2.295
_diffrn_source                   'micro source'
_diffrn_source_type              'Bruker I\mS'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1730 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0292P)²+0.3608P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4219
_reflns_number_total             4490
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt03862c2.cif
_cod_data_source_block           tq036
_cod_depositor_comments
'Adding full bibliography for 7044901--7044905.cif.'
_cod_database_code               7044902
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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
Ca1 Ca 0.61851(4) 0.39649(3) 0.23307(2) 0.01450(11) Uani 1 1 d
C1 C 0.31163(18) 0.53278(16) 0.03860(12) 0.0164(4) Uani 1 1 d
C2 C 0.28790(19) 0.64334(16) 0.04159(12) 0.0169(4) Uani 1 1 d
C3 C 0.21571(19) 0.67008(16) -0.02071(12) 0.0174(5) Uani 1 1 d
C4 C 0.19558(19) 0.57609(16) -0.06259(11) 0.0165(4) Uani 1 1 d
C5 C 0.25560(19) 0.49114(17) -0.02603(11) 0.0159(4) Uani 1 1 d
C6 C 0.3780(2) 0.47401(16) 0.09388(12) 0.0181(4) Uani 1 1 d
C7 C 0.33010(19) 0.71359(17) 0.09912(12) 0.0183(5) Uani 1 1 d
C8 C 0.1651(2) 0.77212(17) -0.03637(12) 0.0193(5) Uani 1 1 d
C9 C 0.1219(2) 0.56916(16) -0.12834(12) 0.0175(4) Uani 1 1 d
C10 C 0.25378(19) 0.38097(17) -0.04681(11) 0.0185(5) Uani 1 1 d
N1 N 0.43094(18) 0.43021(15) 0.13987(11) 0.0242(4) Uani 1 1 d
N2 N 0.36365(18) 0.76753(15) 0.14699(10) 0.0250(4) Uani 1 1 d
N3 N 0.1205(2) 0.85326(15) -0.04861(11) 0.0293(5) Uani 1 1 d
N4 N 0.05917(18) 0.56621(15) -0.17961(11) 0.0234(4) Uani 1 1 d
N5 N 0.25208(19) 0.29187(16) -0.06076(11) 0.0278(5) Uani 1 1 d
O1 O 0.55095(17) 0.22402(14) 0.19764(11) 0.0269(4) Uani 1 1 d
H11 H 0.527(3) 0.181(2) 0.2273(17) 0.035(8) Uiso 1 1 d
H12 H 0.508(4) 0.217(3) 0.160(2) 0.080(13) Uiso 1 1 d
O2 O 0.81670(15) 0.31641(15) 0.22963(11) 0.0271(4) Uani 1 1 d
H21 H 0.865(3) 0.329(3) 0.264(2) 0.057(10) Uiso 1 1 d
H22 H 0.827(3) 0.255(3) 0.2194(18) 0.054(10) Uiso 1 1 d
O3 O 0.73536(19) 0.49213(15) 0.32475(10) 0.0293(4) Uani 1 1 d
H31 H 0.710(4) 0.542(3) 0.352(2) 0.075(13) Uiso 1 1 d
H32 H 0.789(3) 0.470(3) 0.3442(18) 0.044(10) Uiso 1 1 d
O4 O 0.59163(15) 0.58822(13) 0.20845(9) 0.0216(3) Uani 1 1 d
H41 H 0.657(3) 0.623(2) 0.2182(17) 0.048(9) Uiso 1 1 d
H42 H 0.576(3) 0.599(3) 0.1639(19) 0.056(10) Uiso 1 1 d
O5 O 0.69611(16) 0.42136(14) 0.10708(9) 0.0255(4) Uani 1 1 d
H51 H 0.716(3) 0.361(3) 0.085(2) 0.066(11) Uiso 1 1 d
H52 H 0.660(3) 0.454(3) 0.0738(19) 0.058(11) Uiso 1 1 d
C101 C 0.0761(2) 0.45134(17) 0.17079(13) 0.0219(5) Uani 1 1 d
C102 C 0.0124(2) 0.47864(17) 0.10524(13) 0.0208(5) Uani 1 1 d
C103 C -0.00258(19) 0.38524(19) 0.06200(12) 0.0215(5) Uani 1 1 d
C104 C 0.0524(2) 0.29987(17) 0.10087(12) 0.0212(5) Uani 1 1 d
C105 C 0.1017(2) 0.34066(17) 0.16813(13) 0.0216(5) Uani 1 1 d
C106 C 0.1097(2) 0.52421(18) 0.22859(14) 0.0287(5) Uani 1 1 d
C107 C -0.0253(2) 0.58474(19) 0.08632(13) 0.0252(5) Uani 1 1 d
C108 C -0.0592(2) 0.37828(18) -0.00971(13) 0.0239(5) Uani 1 1 d
C109 C 0.0573(2) 0.19081(19) 0.07696(13) 0.0241(5) Uani 1 1 d
C110 C 0.1649(2) 0.28068(18) 0.22333(14) 0.0272(5) Uani 1 1 d
N101 N 0.1364(2) 0.58491(18) 0.27401(13) 0.0462(6) Uani 1 1 d
N102 N -0.0509(2) 0.67077(17) 0.07280(13) 0.0376(5) Uani 1 1 d
N103 N -0.1033(2) 0.37263(17) -0.06816(12) 0.0357(5) Uani 1 1 d
N104 N 0.0609(2) 0.10338(18) 0.05768(12) 0.0354(5) Uani 1 1 d
N105 N 0.2163(2) 0.23123(18) 0.26715(14) 0.0416(5) Uani 1 1 d
O10 O 0.03564(18) 0.88205(19) 0.13945(12) 0.0392(5) Uani 1 1 d
H101 H 0.020(4) 0.932(4) 0.110(2) 0.098(16) Uiso 1 1 d
H102 H 0.015(4) 0.829(3) 0.114(2) 0.088(15) 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 O3 143.58(7) . .
O1 Ca1 O2 84.31(7) . .
O3 Ca1 O2 74.65(7) . .
O1 Ca1 O5 89.01(6) . .
O3 Ca1 O5 111.97(6) . .
O2 Ca1 O5 73.00(6) . .
O1 Ca1 O4 143.53(7) . .
O3 Ca1 O4 72.48(6) . .
O2 Ca1 O4 120.77(6) . .
O5 Ca1 O4 75.65(6) . .
O1 Ca1 N4 94.94(6) . 2_565
O3 Ca1 N4 84.81(7) . 2_565
O2 Ca1 N4 142.44(6) . 2_565
O5 Ca1 N4 144.54(6) . 2_565
O4 Ca1 N4 80.58(6) . 2_565
O1 Ca1 N2 71.72(6) . 4_645
O3 Ca1 N2 73.77(6) . 4_645
O2 Ca1 N2 72.72(6) . 4_645
O5 Ca1 N2 141.98(6) . 4_645
O4 Ca1 N2 137.59(6) . 4_645
N4 Ca1 N2 71.47(6) 2_565 4_645
O1 Ca1 N1 74.69(6) . .
O3 Ca1 N1 139.09(7) . .
O2 Ca1 N1 138.68(7) . .
O5 Ca1 N1 71.48(6) . .
O4 Ca1 N1 69.11(6) . .
N4 Ca1 N1 75.65(6) 2_565 .
N2 Ca1 N1 129.91(6) 4_645 .
C5 C1 C2 108.23(18) . .
C5 C1 C6 126.67(18) . .
C2 C1 C6 125.06(19) . .
C3 C2 C1 108.04(18) . .
C3 C2 C7 127.13(19) . .
C1 C2 C7 124.82(19) . .
C2 C3 C4 107.89(18) . .
C2 C3 C8 126.28(19) . .
C4 C3 C8 125.71(19) . .
C3 C4 C5 108.12(17) . .
C3 C4 C9 124.98(18) . .
C5 C4 C9 126.83(18) . .
C1 C5 C4 107.72(17) . .
C1 C5 C10 125.16(19) . .
C4 C5 C10 126.99(19) . .
N1 C6 C1 177.4(2) . .
N2 C7 C2 177.8(2) . .
N3 C8 C3 177.8(2) . .
N4 C9 C4 177.1(2) . .
N5 C10 C5 177.5(2) . .
C6 N1 Ca1 155.45(17) . .
C7 N2 Ca1 165.31(18) . 4_655
C9 N4 Ca1 161.03(17) . 2_564
Ca1 O1 H11 123(2) . .
Ca1 O1 H12 119(3) . .
H11 O1 H12 106(3) . .
Ca1 O2 H21 119(2) . .
Ca1 O2 H22 122(2) . .
H21 O2 H22 105(3) . .
Ca1 O3 H31 126(3) . .
Ca1 O3 H32 124(2) . .
H31 O3 H32 106(3) . .
Ca1 O4 H41 111(2) . .
Ca1 O4 H42 111(2) . .
H41 O4 H42 107(3) . .
Ca1 O5 H51 113(2) . .
Ca1 O5 H52 124(2) . .
H51 O5 H52 103(3) . .
C102 C101 C105 108.1(2) . .
C102 C101 C106 125.1(2) . .
C105 C101 C106 126.8(2) . .
C101 C102 C103 108.05(19) . .
C101 C102 C107 124.5(2) . .
C103 C102 C107 127.4(2) . .
C102 C103 C104 108.10(19) . .
C102 C103 C108 126.3(2) . .
C104 C103 C108 125.6(2) . .
C105 C104 C103 107.94(19) . .
C105 C104 C109 125.7(2) . .
C103 C104 C109 126.4(2) . .
C104 C105 C101 107.8(2) . .
C104 C105 C110 125.8(2) . .
C101 C105 C110 126.4(2) . .
N101 C106 C101 178.4(3) . .
N102 C107 C102 177.1(3) . .
N103 C108 C103 179.0(2) . .
N104 C109 C104 179.8(3) . .
N105 C110 C105 179.0(3) . .
H101 O10 H102 102(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.3646(17) .
Ca1 O3 2.3949(18) .
Ca1 O2 2.4052(17) .
Ca1 O5 2.4141(16) .
Ca1 O4 2.4524(16) .
Ca1 N4 2.5417(19) 2_565
Ca1 N2 2.6764(19) 4_645
Ca1 N1 2.6823(19) .
C1 C5 1.403(3) .
C1 C2 1.407(3) .
C1 C6 1.427(3) .
C2 C3 1.403(3) .
C2 C7 1.424(3) .
C3 C4 1.407(3) .
C3 C8 1.419(3) .
C4 C5 1.409(3) .
C4 C9 1.425(3) .
C5 C10 1.425(3) .
C6 N1 1.143(3) .
C7 N2 1.146(3) .
C8 N3 1.147(3) .
C9 N4 1.144(3) .
C10 N5 1.140(3) .
N2 Ca1 2.6764(19) 4_655
N4 Ca1 2.5417(19) 2_564
O1 H11 0.80(3) .
O1 H12 0.83(4) .
O2 H21 0.83(4) .
O2 H22 0.80(4) .
O3 H31 0.83(4) .
O3 H32 0.74(4) .
O4 H41 0.86(3) .
O4 H42 0.82(3) .
O5 H51 0.88(4) .
O5 H52 0.82(3) .
C101 C102 1.401(3) .
C101 C105 1.412(3) .
C101 C106 1.421(3) .
C102 C103 1.406(3) .
C102 C107 1.429(3) .
C103 C104 1.408(3) .
C103 C108 1.420(3) .
C104 C105 1.407(3) .
C104 C109 1.428(3) .
C105 C110 1.416(3) .
C106 N101 1.145(3) .
C107 N102 1.137(3) .
C108 N103 1.148(3) .
C109 N104 1.145(3) .
C110 N105 1.144(3) .
O10 H101 0.83(5) .
O10 H102 0.83(4) .
