Amine-Ligated Approach for the Synthesis of Extra-Large-Pore Zinc Phosphites with qtz-h and bnn Topologies.
Wang, Kangcai; Bian, Yixuan; Li, Jing; Xu, Dingguo; Lin, Zhien; Inorganic chemistry 55 (2016) 3727–3729; doi:10.1021/acs.inorgchem.6b00589

data_4347775
_publ_section_title
;
 Amine-Ligated Approach for the Synthesis of Extra-Large-Pore Zinc
 Phosphites with qtz-h and bnn Topologies.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3727
_journal_page_last               3729
_journal_paper_doi               10.1021/acs.inorgchem.6b00589
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C3 H7 N O3 P Zn'
_chemical_formula_sum            'C3 H7 N O3 P Zn'
_chemical_formula_weight         201.44
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
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_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.19880(10)
_cell_length_b                   10.19880(10)
_cell_length_c                   13.4856(3)
_cell_measurement_reflns_used    3131
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.5970
_cell_measurement_theta_min      5.9780
_cell_volume                     1214.78(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000 -150.0000 94

  2 omega  -35.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -19.0000 -180.0000 101

  3 omega   38.00   91.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

  4 omega   38.00   91.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

  5 omega   40.00   98.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 58

  6 omega   91.00  176.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 85

  7 omega   39.00  109.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -150.0000 70

  8 omega  100.00  178.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 78

  9 omega   18.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   38.0000  -60.0000 88

 10 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -180.0000 84

 11 omega   38.00   91.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 12 omega   39.00  109.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 13 omega   70.00  107.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -30.0000 37

 14 omega   87.00  178.00   1.0000    3.2200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0533297000
_diffrn_orient_matrix_UB_12      -0.1703132000
_diffrn_orient_matrix_UB_13      0.0045741000
_diffrn_orient_matrix_UB_21      -0.1613300000
_diffrn_orient_matrix_UB_22      -0.0343235000
_diffrn_orient_matrix_UB_23      0.0257030000
_diffrn_orient_matrix_UB_31      -0.0395117000
_diffrn_orient_matrix_UB_32      -0.0149887000
_diffrn_orient_matrix_UB_33      -0.1112269000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5803
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.912
_diffrn_reflns_theta_max         66.912
_diffrn_reflns_theta_min         5.007
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.694
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.229
_refine_ls_abs_structure_details
;
 Flack x determined using 565 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0669
_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/[\s^2^(Fo^2^)+(0.1420P)^2^+1.6990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.1982
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1410
_reflns_number_total             1444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00589_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        1214.78(4)
_cod_database_code               4347775
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All P(H) groups
2.a Riding coordinates:
 P1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
;
_shelx_res_checksum              27898
_shelx_hkl_checksum              17240
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'