#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/89/4508902.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4508902
loop_
_publ_author_name
'Lin, Zhi-En'
'Fan, Wei'
'Gao, Feifei'
'Chino, Naotaka'
'Yokoi, Toshiyuki'
'Okubo, Tatsuya'
_publ_section_title
;
 A New Organically Templated Zinc Phosphite Synthesized in Phosphorous
 Acid Flux and Its Hydrothermal Analogue
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2435
_journal_paper_doi               10.1021/cg060466e
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C6.5 H9 N O3.5 P Zn'
_chemical_formula_weight         253.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 106.329(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.392(4)
_cell_length_b                   5.199(2)
_cell_length_c                   15.863(6)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      1.96
_cell_volume                     901.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'phi and omega 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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5249
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.877
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6367
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0570P)²+0.0139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                1674
_reflns_number_total             2072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060466esup2.cif
_cod_data_source_block           2
_cod_original_cell_volume        901.5(6)
_cod_original_sg_symbol_H-M      P2/n
_cod_original_formula_sum        'C6.50 H9 N O3.50 P Zn'
_cod_database_code               4508902
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.35842(3) 0.29702(7) 0.50103(2) 0.03274(16) Uani 1 1 d .
P1 P 0.55644(8) 0.22751(16) 0.39517(6) 0.0311(2) Uani 1 1 d .
H1 H 0.550(4) 0.289(7) 0.315(3) 0.049(12) Uiso 1 1 d .
O1 O 0.5741(2) -0.0585(5) 0.40588(15) 0.0468(6) Uani 1 1 d .
O2 O 0.6664(2) 0.3788(5) 0.44710(17) 0.0439(6) Uani 1 1 d .
O3 O 0.4386(2) 0.3233(5) 0.40949(17) 0.0445(6) Uani 1 1 d .
OW1 O 0.2500 0.4947(14) 0.2500 0.122(2) Uani 1 2 d S
N1 N 0.1916(3) 0.1613(6) 0.43018(19) 0.0370(6) Uani 1 1 d .
C1 C 0.1888(3) -0.0351(8) 0.3752(2) 0.0453(9) Uani 1 1 d .
H2 H 0.273(4) -0.117(9) 0.370(2) 0.051(11) Uiso 1 1 d .
C2 C 0.0820(4) -0.1555(8) 0.3314(3) 0.0459(9) Uani 1 1 d .
H3 H 0.093(4) -0.280(9) 0.300(3) 0.061(14) Uiso 1 1 d .
C3 C -0.0271(3) -0.0766(7) 0.3420(2) 0.0404(8) Uani 1 1 d .
C4 C -0.0241(3) 0.1301(8) 0.3969(3) 0.0432(8) Uani 1 1 d .
H4 H -0.090(4) 0.194(8) 0.406(3) 0.044(11) Uiso 1 1 d .
C5 C 0.0850(3) 0.2441(7) 0.4395(2) 0.0408(8) Uani 1 1 d .
H5 H 0.087(4) 0.384(9) 0.478(2) 0.051(11) Uiso 1 1 d .
C6 C -0.1428(4) -0.2177(8) 0.2971(4) 0.0559(12) Uani 1 1 d .
H6 H -0.158(5) -0.297(10) 0.347(4) 0.088(19) Uiso 1 1 d .
H7 H -0.128(4) -0.337(10) 0.261(3) 0.065(15) Uiso 1 1 d .
C7 C -0.2500 -0.0552(10) 0.2500 0.0371(11) Uani 1 2 d S
H8 H -0.270(4) 0.067(10) 0.287(3) 0.077(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 0.0000 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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 Zn1 O3 117.06(11) 3_656 .
O1 Zn1 O2 108.14(11) 3_656 3_666
O3 Zn1 O2 114.63(11) . 3_666
O1 Zn1 N1 108.06(11) 3_656 .
O3 Zn1 N1 100.05(11) . .
O2 Zn1 N1 108.13(11) 3_666 .
O1 P1 O3 113.97(15) . .
O1 P1 O2 112.88(14) . .
O3 P1 O2 112.48(15) . .
O1 P1 H1 108.9(17) . .
O3 P1 H1 105.1(18) . .
O2 P1 H1 102.5(18) . .
P1 O1 Zn1 137.65(15) . 3_656
P1 O2 Zn1 119.22(14) . 3_666
P1 O3 Zn1 136.16(16) . .
C5 N1 C1 117.6(3) . .
C5 N1 Zn1 124.2(2) . .
C1 N1 Zn1 118.1(2) . .
N1 C1 C2 122.3(4) . .
N1 C1 H2 119(2) . .
C2 C1 H2 118(2) . .
C3 C2 C1 120.7(4) . .
C3 C2 H3 126(3) . .
C1 C2 H3 113(3) . .
C2 C3 C4 116.8(3) . .
C2 C3 C6 120.2(4) . .
C4 C3 C6 122.9(4) . .
C5 C4 C3 120.4(4) . .
C5 C4 H4 117(3) . .
C3 C4 H4 122(3) . .
N1 C5 C4 122.2(4) . .
N1 C5 H5 117(2) . .
C4 C5 H5 120(2) . .
C7 C6 C3 116.4(4) . .
C7 C6 H6 110(4) . .
C3 C6 H6 99(4) . .
C7 C6 H7 110(3) . .
C3 C6 H7 110(3) . .
H6 C6 H7 110(5) . .
C6 C7 C6 111.4(5) 2_455 .
C6 C7 H8 113(3) 2_455 .
C6 C7 H8 112(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.916(2) 3_656
Zn1 O3 1.925(3) .
Zn1 O2 1.931(3) 3_666
Zn1 N1 2.042(3) .
P1 O1 1.504(3) .
P1 O3 1.508(3) .
P1 O2 1.512(3) .
P1 H1 1.30(4) .
O1 Zn1 1.916(2) 3_656
O2 Zn1 1.931(2) 3_666
N1 C5 1.336(5) .
N1 C1 1.337(5) .
C1 C2 1.371(5) .
C1 H2 1.07(4) .
C2 C3 1.363(5) .
C2 H3 0.85(5) .
C3 C4 1.378(5) .
C3 C6 1.502(5) .
C4 C5 1.371(5) .
C4 H4 0.88(4) .
C5 H5 0.95(4) .
C6 C7 1.500(5) .
C6 H6 0.96(6) .
C6 H7 0.89(5) .
C7 C6 1.500(5) 2_455
C7 H8 0.94(4) .
