Solvent-free synthesis of new inorganic-organic hybrid solids with finely tuned manganese oxalate structures.
Luan, Lindong; Li, Jing; Yin, Changzhen; Lin, Zhien; Huang, Hui; Dalton transactions (Cambridge, England : 2003) 44 (2015) 5974–5977; doi:10.1039/c5dt00431d

data_7034217
_publ_section_title
;
 Solvent-free synthesis of new inorganic-organic hybrid solids with finely
 tuned manganese oxalate structures.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5974
_journal_page_last               5977
_journal_paper_doi               10.1039/c5dt00431d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C13.5 H24 Mn3 N3 O20 P2'
_chemical_formula_weight         775.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-29 deposited with the CCDC.
2015-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                93.349(2)
_cell_angle_beta                 94.504(3)
_cell_angle_gamma                92.452(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0352(2)
_cell_length_b                   10.1895(2)
_cell_length_c                   16.0266(5)
_cell_measurement_reflns_used    6408
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.0440
_cell_measurement_theta_min      4.3360
_cell_volume                     1304.41(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14041
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         5.01
_exptl_absorpt_coefficient_mu    13.706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41875
_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            yellow
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4655
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+0.9371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                4207
_reflns_number_total             4655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00431d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7034215--7034217.cif.'
_cod_original_cell_volume        1304.40(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C13.50 H24 Mn3 N3 O20 P2'
_cod_database_code               7034217