#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/27/4342765.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_4342765
loop_
_publ_author_name
'Senthil Raja, Duraisamy'
'Lin, Pin-Chun'
'Liu, Wei-Ren'
'Zhan, Jun-Xiang'
'Fu, Xin-Yi'
'Lin, Chia-Her'
_publ_section_title
;
 Multidimensional (0D to 3D) Alkaline-Earth Metal Diphosphonates:
 Synthesis, Structural Diversity, and Luminescence Properties.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4268
_journal_page_last               4278
_journal_paper_doi               10.1021/ic5029993
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C4 H14 Ca0.50 N O7 P2'
_chemical_formula_sum            'C4 H14 Ca0.5 N O7 P2'
_chemical_formula_weight         270.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.893(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.7106(2)
_cell_length_b                   15.3214(7)
_cell_length_c                   12.3862(6)
_cell_measurement_reflns_used    5491
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.2193
_cell_measurement_theta_min      2.6588
_cell_volume                     1056.40(8)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 2008)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9443
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.8506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                2107
_reflns_number_total             2603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5029993_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4342764--4342767.cif.'
_cod_original_formula_sum        'C4 H14 Ca0.50 N O7 P2'
_cod_database_code               4342765
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ca1 Ca 0.5000 0.0000 0.0000 0.01843(14) Uani 1 2 d S
P1 P 0.88713(8) -0.06740(3) -0.16913(4) 0.01720(13) Uani 1 1 d .
P2 P 0.71786(8) 0.12469(3) -0.18876(4) 0.02017(13) Uani 1 1 d .
O1 O 0.1241(2) -0.05163(8) -0.08929(12) 0.0267(3) Uani 1 1 d .
O2 O 0.3124(2) 0.08885(8) 0.11157(11) 0.0232(3) Uani 1 1 d .
O3 O 0.9125(3) -0.13944(8) -0.25527(12) 0.0304(3) Uani 1 1 d .
H1 H 0.8770 -0.1914 -0.2334 0.037 Uiso 1 1 d R
O4 O 0.9426(2) 0.14692(9) -0.09201(12) 0.0292(3) Uani 1 1 d .
H2 H 0.9418 0.1118 -0.0352 0.035 Uiso 1 1 d R
O5 O 0.6878(3) 0.19900(8) -0.26986(12) 0.0296(3) Uani 1 1 d .
O6 O 0.5065(2) 0.10184(8) -0.14103(12) 0.0272(3) Uani 1 1 d .
O7 O 1.0237(3) 0.05384(9) -0.29876(13) 0.0323(3) Uani 1 1 d .
H3 H 1.1508 0.0707 -0.2406 0.039 Uiso 1 1 d R
C1 C 0.8134(3) 0.02966(12) -0.25854(16) 0.0219(4) Uani 1 1 d .
C2 C 0.6141(4) 0.00754(14) -0.35847(18) 0.0363(5) Uani 1 1 d .
H2A H 0.5716 0.0588 -0.4031 0.054 Uiso 1 1 calc R
H2B H 0.4762 -0.0132 -0.3339 0.054 Uiso 1 1 calc R
H2C H 0.6688 -0.0370 -0.4015 0.054 Uiso 1 1 calc R
N1 N 0.8833(3) 0.23376(11) -0.45171(16) 0.0342(4) Uani 1 1 d .
H4 H 0.8346 0.2897 -0.4606 0.041 Uiso 1 1 calc R
H5 H 0.8208 0.2106 -0.3975 0.041 Uiso 1 1 calc R
C3 C 0.7875(6) 0.18623(18) -0.5548(2) 0.0572(7) Uani 1 1 d .
H3A H 0.8326 0.2158 -0.6154 0.086 Uiso 1 1 calc R
H3B H 0.6155 0.1837 -0.5676 0.086 Uiso 1 1 calc R
H3C H 0.8515 0.1281 -0.5489 0.086 Uiso 1 1 calc R
C4 C 1.1465(4) 0.23208(19) -0.4165(3) 0.0584(8) Uani 1 1 d .
H4A H 1.1990 0.1737 -0.3957 0.088 Uiso 1 1 calc R
H4B H 1.1972 0.2703 -0.3542 0.088 Uiso 1 1 calc R
H4C H 1.2154 0.2511 -0.4764 0.088 Uiso 1 1 calc R
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 Ca1 O1 180.0 3_655 .
O1 Ca1 O6 87.80(5) 3_655 .
O1 Ca1 O6 92.21(5) . .
O1 Ca1 O6 92.21(5) 3_655 3_655
O1 Ca1 O6 87.79(5) . 3_655
O6 Ca1 O6 180.0 . 3_655
O1 Ca1 O2 90.96(5) 3_655 .
O1 Ca1 O2 89.04(5) . .
O6 Ca1 O2 97.87(4) . .
O6 Ca1 O2 82.13(4) 3_655 .
O1 Ca1 O2 89.04(5) 3_655 3_655
O1 Ca1 O2 90.96(5) . 3_655
O6 Ca1 O2 82.13(4) . 3_655
O6 Ca1 O2 97.87(4) 3_655 3_655
O2 Ca1 O2 180.0 . 3_655
O1 Ca1 P2 107.44(4) 3_655 3_655
O1 Ca1 P2 72.55(4) . 3_655
O6 Ca1 P2 159.64(3) . 3_655
O6 Ca1 P2 20.36(3) 3_655 3_655
O2 Ca1 P2 69.15(3) . 3_655
O2 Ca1 P2 110.85(3) 3_655 3_655
O1 Ca1 P1 104.65(4) 3_655 3_655
O1 Ca1 P1 75.35(4) . 3_655
O6 Ca1 P1 111.33(3) . 3_655
O6 Ca1 P1 68.67(3) 3_655 3_655
O2 Ca1 P1 19.21(3) . 3_655
O2 Ca1 P1 160.79(3) 3_655 3_655
P2 Ca1 P1 52.539(11) 3_655 3_655
O1 P1 O2 112.78(8) 1_655 3_655
O1 P1 O3 110.75(8) 1_655 .
O2 P1 O3 111.30(7) 3_655 .
O1 P1 C1 108.42(8) 1_655 .
O2 P1 C1 111.33(8) 3_655 .
O3 P1 C1 101.70(8) . .
O6 P2 O5 117.30(8) . .
O6 P2 O4 109.84(8) . .
O5 P2 O4 107.17(8) . .
O6 P2 C1 110.49(8) . .
O5 P2 C1 106.72(8) . .
O4 P2 C1 104.51(8) . .
P1 O1 Ca1 165.05(9) 1_455 .
P1 O2 Ca1 129.81(7) 3_655 .
P1 O3 H1 111.4 . .
P2 O4 H2 108.8 . .
P2 O6 Ca1 126.61(8) . .
C1 O7 H3 111.4 . .
O7 C1 C2 107.73(16) . .
O7 C1 P2 108.38(12) . .
C2 C1 P2 108.23(13) . .
O7 C1 P1 108.48(12) . .
C2 C1 P1 109.75(13) . .
P2 C1 P1 114.09(10) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C4 N1 C3 114.1(2) . .
C4 N1 H4 108.7 . .
C3 N1 H4 108.7 . .
C4 N1 H5 108.7 . .
C3 N1 H5 108.7 . .
H4 N1 H5 107.6 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.3230(13) 3_655
Ca1 O1 2.3230(13) .
Ca1 O6 2.3487(13) .
Ca1 O6 2.3487(13) 3_655
Ca1 O2 2.3605(12) .
Ca1 O2 2.3606(12) 3_655
Ca1 P2 3.4586(5) 3_655
Ca1 P1 3.5226(4) 3_655
P1 O1 1.5070(14) 1_655
P1 O2 1.5088(13) 3_655
P1 O3 1.5643(13) .
P1 C1 1.8459(19) .
P2 O6 1.4990(13) .
P2 O5 1.5026(14) .
P2 O4 1.5853(14) .
P2 C1 1.8371(19) .
O1 P1 1.5070(14) 1_455
O2 P1 1.5088(13) 3_655
O3 H1 0.8797 .
O4 H2 0.8874 .
O7 C1 1.447(2) .
O7 H3 0.9374 .
C1 C2 1.521(3) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
N1 C4 1.469(3) .
N1 C3 1.466(3) .
N1 H4 0.9000 .
N1 H5 0.9000 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
