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_7223191
_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         '0.5(C4 H12 Mg4 O28 P4), C3 N2'
_chemical_formula_sum            'C5 H18 Mg2 N2 O14 P2'
_chemical_formula_weight         440.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-09 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.704(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.4134(2)
_cell_length_b                   15.2590(6)
_cell_length_c                   9.0176(4)
_cell_measurement_reflns_used    1446
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.5900
_cell_measurement_theta_min      3.9990
_cell_volume                     742.37(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -4.00   24.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -17.5174  -99.0000    0.0000 28

  2 omega  -49.00   33.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       19.3143  -57.0000 -150.0000 82

  3 omega  -48.00   40.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       19.3143  -57.0000   90.0000 88

  4 omega  -90.00  -63.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -17.5174  -38.0000  120.0000 27
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1101660000
_diffrn_orient_matrix_UB_12      -0.0246115000
_diffrn_orient_matrix_UB_13      -0.0161169000
_diffrn_orient_matrix_UB_21      0.0508081000
_diffrn_orient_matrix_UB_22      -0.0185091000
_diffrn_orient_matrix_UB_23      -0.0629400000
_diffrn_orient_matrix_UB_31      0.0507135000
_diffrn_orient_matrix_UB_32      -0.0348325000
_diffrn_orient_matrix_UB_33      0.0447538000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3165
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.503
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.972
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0523P)^2^+1.7185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1310
_reflns_number_total             1517
_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               7223191
_chemical_oxdiff_formula         c8h12n4o2mg1
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Sof(N1A)=1-FVAR(1)
 Sof(N1)=FVAR(1)
 Fixed Sof: C3(0.5)
3.a Riding coordinates:
 OW1(HW1A,HW1B)
3.b Tetrahedral OH refined with riding coordinates:
 O4(H4)
;
_shelx_res_checksum              5389
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'