Proton transfer in polyamine-P<sub>2</sub>Mo<sub>5</sub> model adducts: exploring the effect of polyamine cations on their proton conductivity.
Zhang, Shan; Lu, Ying; Sun, Xiuwei; Li, Zhuo; Dang, Tianyi; Liu, Shuxia; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17301–17309; doi:10.1039/d0dt03446k

data_7706124
_publ_section_title
;
 Proton transfer in polyamine-P<sub>2</sub>Mo<sub>5</sub> model adducts:
 exploring the effect of polyamine cations on their proton conductivity.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17301
_journal_page_last               17309
_journal_paper_doi               10.1039/d0dt03446k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'H2 Mo5 O23 P2, 0.5(H2 O), 2(C3 H11 N2)'
_chemical_formula_sum            'C6 H25 Mo5 N4 O23.5 P2'
_chemical_formula_weight         1070.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-09-13 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                84.088(4)
_cell_angle_beta                 77.796(4)
_cell_angle_gamma                65.153(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9361(8)
_cell_length_b                   10.0331(7)
_cell_length_c                   14.4174(12)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    238.22
_cell_measurement_theta_max      32.78
_cell_measurement_theta_min      2.30
_cell_volume                     1274.59(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      238.22
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36069
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.888
_diffrn_reflns_theta_min         2.612
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.628
_exptl_absorpt_correction_T_max  0.9714
_exptl_absorpt_correction_T_min  0.8862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.790
_exptl_crystal_description       block
_exptl_crystal_F_000             1034
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0227P)^2^+2.8736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6191
_reflns_number_total             8779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03446k2.cif
_cod_data_source_block           TETA
_cod_original_formula_sum        'C6 H25 Mo5 N4 O23.50 P2'
_cod_database_code               7706124
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), N4(H4A,H4B), C1(H1D,H1E),
 C2(H2C,H2D), C4(H4C,H4D)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N3(H3C,H3D,H3E)
3.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O18(H18)
;
_shelx_res_checksum              41329
_olex2_submission_special_instructions 'No special instructions were received'