Solvent-free synthesis of new magnesium phosphate‒oxalates displaying diverse framework topologies
Zhang, Wei; Kang, Maoping; Yang, Meng; Luo, Daibing; Lin, Zhien; CrystEngComm 17 (2015) 9296–; doi:10.1039/C5CE02001H

data_7223193
_publ_section_title
;
 Solvent-free synthesis of new magnesium phosphate--oxalates displaying
 diverse framework topologies
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              9296
_journal_paper_doi               10.1039/C5CE02001H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         '0.25(C16 H16 Mg8 O64 P8), C4 H14 N2'
_chemical_formula_sum            'C8 H18 Mg2 N2 O16 P2'
_chemical_formula_weight         508.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-13 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.23203(11)
_cell_length_b                   16.34232(15)
_cell_length_c                   13.28134(15)
_cell_measurement_reflns_used    4937
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.4810
_cell_measurement_theta_min      5.4200
_cell_volume                     1786.74(4)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_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    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000 -180.0000 74

  2 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  -60.0000 84

  3 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  -90.0000 74

  4 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -120.0000 94

  5 omega   87.00  178.00   1.0000    3.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 91

  6 omega   38.00   91.00   1.0000    3.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

  7 omega   38.00   91.00   1.0000    3.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

  8 omega  100.00  178.00   1.0000    3.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 78

  9 omega   39.00  109.00   1.0000    3.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 10 omega   40.00   98.00   1.0000    3.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

 11 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   30.0000 94

 12 omega   18.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   38.0000    0.0000 88

 13 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000   30.0000 84

 14 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  150.0000 84

 15 omega   39.00   64.00   1.0000    3.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  150.0000 25

 16 omega   87.00  178.00   1.0000    3.7400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 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      0.0159145000
_diffrn_orient_matrix_UB_12      -0.0785586000
_diffrn_orient_matrix_UB_13      0.0633359000
_diffrn_orient_matrix_UB_21      -0.0284066000
_diffrn_orient_matrix_UB_22      0.0500390000
_diffrn_orient_matrix_UB_23      0.0967066000
_diffrn_orient_matrix_UB_31      -0.1843178000
_diffrn_orient_matrix_UB_32      -0.0144952000
_diffrn_orient_matrix_UB_33      -0.0094066000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8378
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.056
_diffrn_reflns_theta_max         67.056
_diffrn_reflns_theta_min         5.414
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.788
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49625
_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    1.891
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         1594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+2.6758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1497
_reflns_number_total             1594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02001h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7223190--7223197.cif.'
_cod_database_code               7223193
_reflns_odcompleteness_completeness 99.84
_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 C(H,H,H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C5')
3. Others
 Sof(H4BC)=Sof(H4BD)=Sof(C5')=Sof(H5'A)=Sof(H5'B)=1-FVAR(1)
 Sof(H4AB)=Sof(H4AA)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AB,H4AA), C5(H5A,H5B), C5'(H5'A,H5'B)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
4.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_shelx_res_checksum              97814
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'