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_7223197
_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         'C4 H5 Mg2 O17 P2, H2 O, O, C6 H20 N3'
_chemical_formula_sum            'C10 H29 Mg2 N3 O19 P2'
_chemical_formula_weight         605.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-19
_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                96.449(2)
_cell_angle_beta                 103.879(2)
_cell_angle_gamma                104.350(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3254(2)
_cell_length_b                   9.4280(3)
_cell_length_c                   14.3060(4)
_cell_measurement_reflns_used    11600
_cell_measurement_temperature    292.8(4)
_cell_measurement_theta_max      72.5130
_cell_measurement_theta_min      4.9150
_cell_volume                     1163.07(6)
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.8(4)
_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   23.00   90.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000    0.0000 67

  2 omega  -33.00   55.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000    0.0000 88

  3 omega   20.00  104.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -30.0000 84

  4 omega  -31.00   63.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000  120.0000 94

  5 omega  -33.00   55.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000  150.0000 88

  6 omega    1.00   75.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000   60.0000 74

  7 omega   10.00  104.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -150.0000 94

  8 omega   20.00  104.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -60.0000 84

  9 omega   38.00   91.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 10 omega   40.00   98.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

 11 omega   39.00  109.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  150.0000 70

 12 omega   40.00  135.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 95

 13 omega   37.00  146.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 109

 14 omega   38.00   91.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

 15 omega   38.00   91.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

 16 omega   38.00  116.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 78

 17 omega   39.00  109.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 70

 18 omega   38.00   91.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 19 omega   39.00  109.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 70

 20 omega  101.00  178.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   96.0000  -44.0000 77

 21 omega   91.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 85

 22 omega   70.00  178.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   90.0000 108

 23 omega   10.00  104.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  -30.0000 94

 24 omega   10.00  104.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  150.0000 94

 25 omega   18.00  106.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   38.0000 -180.0000 88

 26 omega   10.00  104.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   30.0000 94

 27 omega   23.00   90.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000 -150.0000 67

 28 omega  -33.00   55.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000 -120.0000 88

 29 omega   10.00  104.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   90.0000 94

 30 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95

 31 omega   91.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 85

 32 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

 33 omega   91.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 85

 34 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95

 35 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 95

 36 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95

 37 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 95

 38 omega   87.00  178.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000    0.0000 91

 39 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 95

 40 omega   90.00  175.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  150.0000 85

 41 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

 42 omega   81.00  176.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

 43 omega   70.00  178.00   1.0000   10.7700
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 108

 44 omega    7.00  108.00   1.0000    2.6900
omega____ theta____ kappa____ phi______ frames
    -       36.5421   19.0000 -180.0000 101
;
_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      0.1698326000
_diffrn_orient_matrix_UB_12      0.0880982000
_diffrn_orient_matrix_UB_13      0.0172700000
_diffrn_orient_matrix_UB_21      0.0054471000
_diffrn_orient_matrix_UB_22      0.0696220000
_diffrn_orient_matrix_UB_23      0.1039605000
_diffrn_orient_matrix_UB_31      0.0513994000
_diffrn_orient_matrix_UB_32      -0.1296952000
_diffrn_orient_matrix_UB_33      0.0402845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20658
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         4.925
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78058
_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    1.730
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0995P)^2^+0.3362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3852
_reflns_number_total             4163
_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               7223197
_reflns_odcompleteness_completeness 99.98
_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 N(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Sof(OW3')=1-FVAR(1)
 Sof(OW3)=FVAR(1)
3.a Riding coordinates:
 OW1(HW1A,HW1B), OW2(HW2A,HW2B)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B)
3.c Me refined with riding coordinates:
 N1(H1A,H1B,H1C), N3(H3A,H3B,H3C)
3.d Tetrahedral OH refined with riding coordinates:
 O4(H4), O6(H6), O7(H7)
;
_shelx_res_checksum              87301
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'