#------------------------------------------------------------------------------
#$Date: 2009-11-21 12:50:34 +0200 (Sat, 21 Nov 2009) $
#$Revision: 900 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1004030.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_1004030

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C5 H17 N O10 P2 Zn'
_chemical_formula_weight          378.51
_chemical_melting_point           ?
_chemical_compound_source         ?

_publ_section_title
;
Synthesis and characterization of Mu-19, a new zincophosphate with a three
dimensional 12-membered ring channel system
;
loop_
_publ_author_name
  'Simon, L. Josien, V. Gramlich, J. Patarin'
_journal_name_full                 'Microporous Mesoporous Mater. 2001, 47, 135'

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'
 'Zn'  'Zn'   0.2839   1.4301
 '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'

_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    P2(1)2(1)2(1)

loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'

_cell_length_a                    9.976(4)
_cell_length_b                    10.359(6)
_cell_length_c                    12.980(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1341.4(14)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     12
_cell_measurement_theta_min       10
_cell_measurement_theta_max       11

_exptl_crystal_description        'prism'
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.3
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.874
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              776
_exptl_absorpt_coefficient_mu     2.115
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        'SYNTEX P21 4-circle diffractometer'
_diffrn_measurement_method        ' \w scans'
_diffrn_standards_number          1
_diffrn_standards_interval_count  120
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             752
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0206
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          2.52
_diffrn_reflns_theta_max          20.04
_reflns_number_total              752
_reflns_number_observed           713
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'SIEMENS SHELXTL Plus'
_computing_cell_refinement        'SIEMENS SHELXTL Plus'
_computing_data_reduction         'SIEMENS SHELXTL Plus'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     SHELXLTL-Plus
_computing_publication_material   SHELXL-93

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
 or flagged by the user for potential systematic errors.  Weighted R-factors
 wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
 are based on F, with F set to zero for negative F^2^. The observed criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.8291P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0109(13)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.02(2)
_refine_ls_number_reflns          752
_refine_ls_number_parameters      173
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0233
_refine_ls_R_factor_obs           0.0222
_refine_ls_wR_factor_all          0.0572
_refine_ls_wR_factor_obs          0.0569
_refine_ls_goodness_of_fit_all    1.126
_refine_ls_goodness_of_fit_obs    1.159
_refine_ls_restrained_S_all       1.126
_refine_ls_restrained_S_obs       1.159
_refine_ls_shift/esd_max          0.001
_refine_ls_shift/esd_mean         0.000

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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Zn Zn 0.97152(7) 0.20187(7) 0.63523(5) 0.0175(3) Uani 1 d . .
P2 P 0.8895(2) 0.4399(2) 0.78593(13) 0.0211(5) Uani 1 d . .
P1 P 1.2264(2) 0.2147(2) 0.49650(14) 0.0215(5) Uani 1 d . .
O6 O 0.8199(5) 0.5137(4) 0.6964(4) 0.0459(15) Uani 1 d . .
H6 H 0.7595(5) 0.4610(4) 0.6390(4) 0.102 Uiso 1 d R .
O2 O 1.1220(4) 0.2759(4) 0.5657(3) 0.0259(12) Uani 1 d . .
O1 O 0.9357(4) 0.3098(4) 0.7519(3) 0.0258(11) Uani 1 d . .
O7 O 1.3107(5) 0.1137(4) 0.5479(4) 0.0310(13) Uani 1 d . .
O5 O 0.7847(5) 0.4175(4) 0.8698(4) 0.0429(14) Uani 1 d . .
H5 H 0.7423(5) 0.4809(4) 0.9177(4) 0.050 Uiso 1 d R .
O3 O 1.0010(4) 0.0259(4) 0.6783(3) 0.0268(12) Uani 1 d . .
O4 O 0.8122(4) 0.1789(4) 0.5506(3) 0.0232(11) Uani 1 d . .
O8 O 1.1509(4) 0.1421(4) 0.4062(3) 0.0335(13) Uani 1 d . .
H8 H 1.0841(4) 0.2021(4) 0.3612(3) 0.114 Uiso 1 d R .
C6 C 0.7656(7) -0.1778(8) 0.6289(6) 0.043(2) Uani 1 d . .
H6A H 0.8074(7) -0.2482(8) 0.6647(6) 0.061 Uiso 1 d R .
H6B H 0.7852(7) -0.0993(8) 0.6653(6) 0.061 Uiso 1 d R .
C3 C 0.6055(8) -0.0789(8) 0.4695(6) 0.048(2) Uani 1 d . .
H3A H 0.5818(8) -0.1552(8) 0.4317(6) 0.067 Uiso 1 d R .
H3B H 0.5616(8) -0.0064(8) 0.4381(6) 0.067 Uiso 1 d R .
C5 C 0.8194(7) -0.1678(7) 0.5214(6) 0.043(2) Uani 1 d . .
H5A H 0.9147(7) -0.1545(7) 0.5220(6) 0.061 Uiso 1 d R .
H5B H 0.8014(7) -0.2474(7) 0.4862(6) 0.061 Uiso 1 d R .
C2 C 0.5617(7) -0.0923(8) 0.5784(6) 0.043(2) Uani 1 d . .
H2A H 0.5835(7) -0.0151(8) 0.6156(6) 0.061 Uiso 1 d R .
H2B H 0.4663(7) -0.1043(8) 0.5813(6) 0.061 Uiso 1 d R .
N N 0.7537(7) -0.0607(6) 0.4655(4) 0.037(2) Uani 1 d . .
H0A H 0.7730(7) 0.0130(6) 0.4990(4) 0.051 Uiso 1 d R .
C7 C 0.8023(12) -0.0476(9) 0.3585(6) 0.086(4) Uani 1 d . .
H7A H 0.7563(12) 0.0236(9) 0.3269(6) 0.120 Uiso 1 d R .
H7D H 0.7825(12) -0.1255(9) 0.3215(6) 0.120 Uiso 1 d R .
H7B H 0.8971(12) -0.0320(9) 0.3570(6) 0.120 Uiso 1 d R .
O O 0.6249(5) -0.1982(5) 0.6258(4) 0.0476(14) Uani 1 d . .
O1W O 1.4862(5) 0.2090(5) 0.6907(4) 0.0492(14) Uani 1 d . .
H1 H 1.4087(5) 0.2008(5) 0.6413(4) 0.069 Uiso 1 d R .
H2 H 1.4390(5) 0.2230(5) 0.7799(4) 0.387 Uiso 1 d R .

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Zn 0.0203(5) 0.0125(5) 0.0196(5) 0.0003(4) 0.0003(3) 0.0012(4)
P2 0.0260(10) 0.0131(10) 0.0241(10) -0.0021(9) 0.0000(9) -0.0006(9)
P1 0.0227(10) 0.0176(11) 0.0243(9) 0.0011(11) 0.0052(9) -0.0021(10)
O6 0.069(4) 0.027(3) 0.042(3) -0.003(3) -0.027(3) 0.002(3)
O2 0.022(2) 0.028(3) 0.028(3) -0.002(2) 0.010(2) -0.001(2)
O1 0.040(3) 0.015(3) 0.023(2) -0.008(2) 0.006(2) 0.001(3)
O7 0.028(3) 0.023(3) 0.042(3) 0.013(2) 0.002(3) 0.000(2)
O5 0.051(3) 0.021(3) 0.057(3) -0.013(3) 0.039(3) -0.008(3)
O3 0.025(3) 0.010(2) 0.046(3) 0.010(2) -0.003(2) 0.004(2)
O4 0.027(3) 0.014(3) 0.029(3) 0.000(2) -0.008(2) 0.004(2)
O8 0.038(3) 0.028(3) 0.034(3) -0.007(2) 0.005(3) -0.007(3)
C6 0.040(5) 0.040(5) 0.050(5) 0.019(5) -0.007(4) -0.001(4)
C3 0.052(6) 0.026(5) 0.065(6) 0.004(4) -0.030(5) -0.003(4)
C5 0.032(4) 0.032(5) 0.066(6) -0.012(5) 0.001(5) 0.001(4)
C2 0.025(4) 0.031(5) 0.074(6) 0.003(5) 0.004(5) 0.002(4)
N 0.061(5) 0.018(3) 0.030(3) -0.006(3) 0.000(4) -0.006(4)
C7 0.154(11) 0.064(7) 0.039(5) -0.013(6) 0.027(7) -0.025(8)
O 0.047(4) 0.043(3) 0.052(3) 0.010(3) 0.009(3) -0.007(3)
O1W 0.044(3) 0.061(3) 0.042(3) -0.001(3) 0.005(3) -0.010(4)


_refine_diff_density_max    0.258
_refine_diff_density_min   -0.290
_refine_diff_density_rms    0.056