Solvent-free synthesis of crystalline metal phosphate oxalates with a (4,6)-connected fsh topology.
Luan, Lindong; Li, Jing; Chen, Cheng; Lin, Zhien; Huang, Hui; Inorganic chemistry 54 (2015) 9387–9389; doi:10.1021/acs.inorgchem.5b01569

data_4346480
_publ_section_title
;
 Solvent-free synthesis of crystalline metal phosphate oxalates with a
 (4,6)-connected fsh topology.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9387
_journal_page_last               9389
_journal_paper_doi               10.1021/acs.inorgchem.5b01569
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C4 H3 Mn2 O14 P1.5, C5 H14 N1.5, H2 O'
_chemical_formula_sum            'C9 H19 Mn2 N1.5 O15 P1.5'
_chemical_formula_weight         544.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-13
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_cell_angle_gamma                90
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_cell_length_a                   15.3680(4)
_cell_length_b                   11.4122(3)
_cell_length_c                   22.2812(5)
_cell_measurement_reflns_used    5447
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.9370
_cell_measurement_theta_min      3.6980
_cell_volume                     3824.50(17)
_computing_cell_refinement
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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_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)
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_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)
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_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -54.00   34.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -       15.5694  -38.0000  -60.0000 88

  2 omega   -1.00   83.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -       15.5694   57.0000  120.0000 84

  3 omega  -84.00   10.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.6631  -77.0000  120.0000 94

  4 omega  -79.00  -32.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -      -16.6631  141.0000  -70.0000 47

  5 omega  -20.00    5.00   1.0000    4.3800
omega____ theta____ kappa____ phi______ frames
    -       15.5694  -99.0000 -180.0000 25
;
_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      0.0403662000
_diffrn_orient_matrix_UB_12      -0.0099875000
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_diffrn_orient_matrix_UB_21      -0.0076651000
_diffrn_orient_matrix_UB_22      -0.0612724000
_diffrn_orient_matrix_UB_23      0.0001622000
_diffrn_orient_matrix_UB_31      -0.0231223000
_diffrn_orient_matrix_UB_32      0.0028575000
_diffrn_orient_matrix_UB_33      -0.0309851000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12442
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.364
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description
;
;
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.469
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_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0411
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+15.2239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3371
_reflns_number_total             3901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01569_si_003.cif
_cod_data_source_block           1
_cod_original_cell_volume        3824.52(16)
_cod_original_formula_sum        'C9 H19 Mn2 N1.50 O15 P1.50'
_cod_database_code               4346480
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 N2(H2), OW1(HW1A,HW1B)
2.b Ternary CH refined with riding coordinates:
 N1(H1)
2.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O6(H6)
;
_shelx_res_checksum              56330
_shelx_hkl_checksum              27151
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'