#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:28:49 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179665 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/18/4511885.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_4511885
loop_
_publ_author_name
'Demadis, Konstantinos D.'
'Armakola, Eirini'
'Papathanasiou, Konstantinos E.'
'Mezei, Gellert'
'Kirillov, Alexander M.'
_publ_section_title
;
 Structural Systematics and Topological Analysis of Coordination Polymers
 with Divalent Metals and a Glycine-Derived Tripodal Phosphonocarboxylate
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5234
_journal_paper_doi               10.1021/cg501029b
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C4 H11 Ca N O9 P2'
_chemical_formula_weight         319.16
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                78.615(5)
_cell_angle_beta                 80.272(5)
_cell_angle_gamma                88.585(5)
_cell_formula_units_Z            2
_cell_length_a                   7.1200(4)
_cell_length_b                   7.2986(5)
_cell_length_c                   10.5043(6)
_cell_measurement_reflns_used    1441
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.29
_cell_measurement_theta_min      2.90
_cell_volume                     527.41(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11139
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.006
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       prism
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2074
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0417
_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)+(0.0502P)²+0.3667P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1622
_reflns_number_total             2074
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg501029b_si_002.cif
_cod_data_source_block           CaBPMGLY
_cod_depositor_comments
'Adding full bibliography for 4511884--4511887.cif.'
_cod_database_code               4511885
#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.
;
_shelx_estimated_absorpt_t_min   0.766
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
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
P1 P 0.52072(12) 0.27358(12) 0.88291(9) 0.0157(2) Uani 1 1 d . .
P2 P 0.11216(12) -0.11596(12) 0.78868(9) 0.0173(2) Uani 1 1 d . .
Ca1 Ca 0.62332(9) -0.17881(9) 0.74901(7) 0.0141(2) Uani 1 1 d . .
O1 O 0.6024(4) 0.1128(3) 0.8243(3) 0.0235(6) Uani 1 1 d . .
O2 O 0.5323(3) 0.2703(3) 1.0242(2) 0.0202(6) Uani 1 1 d . .
O3 O 0.6102(4) 0.4614(3) 0.7954(2) 0.0208(6) Uani 1 1 d D .
H3 H 0.660(5) 0.441(5) 0.724(3) 0.025 Uiso 1 1 d D U
O4 O 0.3042(3) -0.1488(3) 0.7115(2) 0.0211(6) Uani 1 1 d . .
O5 O 0.1264(4) -0.1573(4) 0.9384(3) 0.0275(6) Uani 1 1 d D .
H5 H 0.232(4) -0.198(6) 0.948(4) 0.033 Uiso 1 1 d D U
O6 O -0.0595(3) -0.2111(3) 0.7675(3) 0.0256(6) Uani 1 1 d . .
O7 O 0.3299(4) 0.2864(4) 0.4699(3) 0.0310(7) Uani 1 1 d . .
O8 O 0.2152(4) 0.5730(3) 0.4252(3) 0.0262(6) Uani 1 1 d . .
O9 O 0.6963(5) 0.0661(4) 0.5642(3) 0.0429(9) Uani 1 1 d D .
H9A H 0.723(7) 0.169(4) 0.571(5) 0.051 Uiso 1 1 d D U
H9B H 0.691(8) 0.065(7) 0.486(2) 0.051 Uiso 1 1 d D U
N1 N 0.2383(4) 0.2565(4) 0.7354(3) 0.0170(6) Uani 1 1 d D .
H1 H 0.338(4) 0.203(5) 0.701(4) 0.020 Uiso 1 1 d D U
C1 C 0.2702(5) 0.2799(5) 0.8704(3) 0.0201(8) Uani 1 1 d . .
H1A H 0.2035 0.1808 0.9368 0.024 Uiso 1 1 calc R U
H1B H 0.2176 0.3982 0.8875 0.024 Uiso 1 1 calc R U
C2 C 0.0674(5) 0.1334(5) 0.7437(4) 0.0194(8) Uani 1 1 d . .
H2A H 0.0248 0.1582 0.6590 0.023 Uiso 1 1 calc R U
H2B H -0.0351 0.1670 0.8081 0.023 Uiso 1 1 calc R U
C3 C 0.2213(5) 0.4406(5) 0.6476(4) 0.0208(8) Uani 1 1 d . .
H3A H 0.3123 0.5276 0.6623 0.025 Uiso 1 1 calc R U
H3B H 0.0946 0.4892 0.6699 0.025 Uiso 1 1 calc R U
C4 C 0.2566(5) 0.4274(5) 0.5039(4) 0.0192(8) Uani 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 0.0000 0.0000 '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'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 '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 P1 O2 117.92(15) . .
O1 P1 O3 109.43(14) . .
O2 P1 O3 109.58(14) . .
O1 P1 C1 106.36(16) . .
O2 P1 C1 106.68(15) . .
O3 P1 C1 106.18(16) . .
O6 P2 O4 119.44(15) . .
O6 P2 O5 109.78(16) . .
O4 P2 O5 108.61(14) . .
O6 P2 C2 105.47(15) . .
O4 P2 C2 106.07(16) . .
O5 P2 C2 106.69(16) . .
O6 Ca1 O9 90.98(12) 1_655 .
O6 Ca1 O4 175.22(9) 1_655 .
O9 Ca1 O4 86.25(11) . .
O6 Ca1 O1 92.31(9) 1_655 .
O9 Ca1 O1 71.56(10) . .
O4 Ca1 O1 90.51(9) . .
O6 Ca1 O2 102.19(9) 1_655 2_657
O9 Ca1 O2 146.80(10) . 2_657
O4 Ca1 O2 82.19(8) . 2_657
O1 Ca1 O2 77.51(9) . 2_657
O6 Ca1 O7 93.38(10) 1_655 2_656
O9 Ca1 O7 66.23(9) . 2_656
O4 Ca1 O7 81.94(9) . 2_656
O1 Ca1 O7 137.47(9) . 2_656
O2 Ca1 O7 141.39(9) 2_657 2_656
O6 Ca1 O3 85.97(8) 1_655 1_545
O9 Ca1 O3 137.41(10) . 1_545
O4 Ca1 O3 93.42(8) . 1_545
O1 Ca1 O3 150.94(9) . 1_545
O2 Ca1 O3 74.54(8) 2_657 1_545
O7 Ca1 O3 71.56(8) 2_656 1_545
P1 O1 Ca1 160.64(16) . .
P1 O2 Ca1 146.13(15) . 2_657
P1 O3 Ca1 149.02(14) . 1_565
P1 O3 H3 109(3) . .
Ca1 O3 H3 100(3) 1_565 .
P2 O4 Ca1 137.15(15) . .
P2 O5 H5 109(3) . .
P2 O6 Ca1 145.11(15) . 1_455
C4 O7 Ca1 131.8(2) . 2_656
Ca1 O9 H9A 122(4) . .
Ca1 O9 H9B 128(4) . .
H9A O9 H9B 109(5) . .
C3 N1 C2 110.9(3) . .
C3 N1 C1 111.3(3) . .
C2 N1 C1 111.9(3) . .
C3 N1 H1 107(3) . .
C2 N1 H1 108(3) . .
C1 N1 H1 107(3) . .
N1 C1 P1 111.7(2) . .
N1 C1 H1A 109.3 . .
P1 C1 H1A 109.3 . .
N1 C1 H1B 109.3 . .
P1 C1 H1B 109.3 . .
H1A C1 H1B 107.9 . .
N1 C2 P2 114.2(2) . .
N1 C2 H2A 108.7 . .
P2 C2 H2A 108.7 . .
N1 C2 H2B 108.7 . .
P2 C2 H2B 108.7 . .
H2A C2 H2B 107.6 . .
N1 C3 C4 112.3(3) . .
N1 C3 H3A 109.2 . .
C4 C3 H3A 109.2 . .
N1 C3 H3B 109.2 . .
C4 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
O7 C4 O8 124.7(3) . .
O7 C4 C3 119.9(3) . .
O8 C4 C3 115.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1 1.491(2) .
P1 O2 1.496(3) .
P1 O3 1.575(3) .
P1 C1 1.809(4) .
P2 O6 1.490(2) .
P2 O4 1.507(2) .
P2 O5 1.562(3) .
P2 C2 1.822(4) .
Ca1 O6 2.301(2) 1_655
Ca1 O9 2.359(3) .
Ca1 O4 2.368(2) .
Ca1 O1 2.406(2) .
Ca1 O2 2.422(3) 2_657
Ca1 O7 2.541(3) 2_656
Ca1 O3 2.575(2) 1_545
O2 Ca1 2.422(3) 2_657
O3 Ca1 2.575(2) 1_565
O3 H3 0.817(19) .
O5 H5 0.817(19) .
O6 Ca1 2.301(2) 1_455
O7 C4 1.231(4) .
O7 Ca1 2.541(3) 2_656
O8 C4 1.273(4) .
O9 H9A 0.799(19) .
O9 H9B 0.827(19) .
N1 C3 1.487(5) .
N1 C2 1.511(4) .
N1 C1 1.516(4) .
N1 H1 0.863(19) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.509(5) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
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
C3 H3B O8 0.97 2.65 3.331(4) 127.3 2_566
C3 H3A O4 0.97 2.51 3.286(4) 136.7 1_565
C2 H2B O5 0.97 2.62 3.427(5) 140.9 2_557
C2 H2B O1 0.97 2.59 3.276(4) 127.6 1_455
C1 H1A O5 0.97 2.48 3.210(4) 131.9 2_557
C1 H1A O5 0.97 2.54 3.279(5) 133.3 .
N1 H1 O4 0.863(19) 2.56(3) 3.036(4) 116(3) .
N1 H1 O1 0.863(19) 2.46(4) 2.997(4) 121(3) .
O9 H9B O4 0.827(19) 2.04(3) 2.841(4) 162(5) 2_656
O9 H9A O8 0.799(19) 1.95(2) 2.751(4) 176(5) 2_666
O5 H5 O2 0.817(19) 1.80(2) 2.615(3) 175(4) 2_657
O3 H3 O8 0.817(19) 1.68(2) 2.493(4) 171(4) 2_666
O3 H3 O7 0.817(19) 2.54(4) 2.991(4) 116(3) 2_666
C3 H3B O8 0.97 2.65 3.331(4) 127.3 2_566
C3 H3A O4 0.97 2.51 3.286(4) 136.7 1_565
C2 H2B O5 0.97 2.62 3.427(5) 140.9 2_557
C2 H2B O1 0.97 2.59 3.276(4) 127.6 1_455
C1 H1A O5 0.97 2.48 3.210(4) 131.9 2_557
C1 H1A O5 0.97 2.54 3.279(5) 133.3 .
N1 H1 O4 0.863(19) 2.56(3) 3.036(4) 116(3) .
N1 H1 O1 0.863(19) 2.46(4) 2.997(4) 121(3) .
O9 H9B O4 0.827(19) 2.04(3) 2.841(4) 162(5) 2_656
O9 H9A O8 0.799(19) 1.95(2) 2.751(4) 176(5) 2_666
O5 H5 O2 0.817(19) 1.80(2) 2.615(3) 175(4) 2_657
O3 H3 O8 0.817(19) 1.68(2) 2.493(4) 171(4) 2_666
O3 H3 O7 0.817(19) 2.54(4) 2.991(4) 116(3) 2_666
O3 H3 O7 0.817(19) 2.54(4) 2.991(4) 116(3) 2_666
O3 H3 O8 0.817(19) 1.68(2) 2.493(4) 171(4) 2_666
O5 H5 O2 0.817(19) 1.80(2) 2.615(3) 175(4) 2_657
O9 H9A O8 0.799(19) 1.95(2) 2.751(4) 176(5) 2_666
O9 H9B O4 0.827(19) 2.04(3) 2.841(4) 162(5) 2_656
N1 H1 O1 0.863(19) 2.46(4) 2.997(4) 121(3) .
N1 H1 O4 0.863(19) 2.56(3) 3.036(4) 116(3) .
C1 H1A O5 0.97 2.54 3.279(5) 133.3 .
C1 H1A O5 0.97 2.48 3.210(4) 131.9 2_557
C2 H2B O1 0.97 2.59 3.276(4) 127.6 1_455
C2 H2B O5 0.97 2.62 3.427(5) 140.9 2_557
C3 H3A O4 0.97 2.51 3.286(4) 136.7 1_565
C3 H3B O8 0.97 2.65 3.331(4) 127.3 2_566
O3 H3 O7 0.817(19) 2.54(4) 2.991(4) 116(3) 2_666
O3 H3 O8 0.817(19) 1.68(2) 2.493(4) 171(4) 2_666
O5 H5 O2 0.817(19) 1.80(2) 2.615(3) 175(4) 2_657
O9 H9A O8 0.799(19) 1.95(2) 2.751(4) 176(5) 2_666
O9 H9B O4 0.827(19) 2.04(3) 2.841(4) 162(5) 2_656
N1 H1 O1 0.863(19) 2.46(4) 2.997(4) 121(3) .
N1 H1 O4 0.863(19) 2.56(3) 3.036(4) 116(3) .
C1 H1A O5 0.97 2.54 3.279(5) 133.3 .
C1 H1A O5 0.97 2.48 3.210(4) 131.9 2_557
C2 H2B O1 0.97 2.59 3.276(4) 127.6 1_455
C2 H2B O5 0.97 2.62 3.427(5) 140.9 2_557
C3 H3A O4 0.97 2.51 3.286(4) 136.7 1_565
C3 H3B O8 0.97 2.65 3.331(4) 127.3 2_566
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_4
O2 P1 O1 Ca1 96.5(5) . .
O3 P1 O1 Ca1 -137.5(5) . .
C1 P1 O1 Ca1 -23.2(5) . .
O1 P1 O2 Ca1 -90.7(3) . 2_657
O3 P1 O2 Ca1 143.3(2) . 2_657
C1 P1 O2 Ca1 28.7(3) . 2_657
O1 P1 O3 Ca1 176.2(3) . 1_565
O2 P1 O3 Ca1 -53.1(3) . 1_565
C1 P1 O3 Ca1 61.8(3) . 1_565
O6 P2 O4 Ca1 -143.7(2) . .
O5 P2 O4 Ca1 -16.8(3) . .
C2 P2 O4 Ca1 97.5(2) . .
O4 P2 O6 Ca1 -140.5(3) . 1_455
O5 P2 O6 Ca1 93.2(3) . 1_455
C2 P2 O6 Ca1 -21.4(3) . 1_455
C3 N1 C1 P1 -95.3(3) . .
C2 N1 C1 P1 139.9(2) . .
O1 P1 C1 N1 -45.4(3) . .
O2 P1 C1 N1 -172.1(2) . .
O3 P1 C1 N1 71.1(3) . .
C3 N1 C2 P2 156.1(2) . .
C1 N1 C2 P2 -79.0(3) . .
O6 P2 C2 N1 -170.0(2) . .
O4 P2 C2 N1 -42.4(3) . .
O5 P2 C2 N1 73.3(3) . .
C2 N1 C3 C4 -74.3(4) . .
C1 N1 C3 C4 160.5(3) . .
Ca1 O7 C4 O8 -13.5(6) 2_656 .
Ca1 O7 C4 C3 170.5(2) 2_656 .
N1 C3 C4 O7 -14.1(5) . .
N1 C3 C4 O8 169.5(3) . .
