Homoleptic borates and aluminates containing the difluorophosphato ligand - [M(O2PF2)x](y-) - synthesis and characterization.
Schulz, Christoph; Eiden, Philipp; Klose, Petra; Ermantraut, Andreas; Schmidt, Michael; Garsuch, Arnd; Krossing, Ingo; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7048–7057; doi:10.1039/c5dt00469a

data_7034458
_publ_section_title
;
 Homoleptic borates and aluminates containing the difluorophosphato ligand
 - [M(O2PF2)x](y-) - synthesis and characterization.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7048
_journal_page_last               7057
_journal_paper_doi               10.1039/c5dt00469a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'0.5(C24 H60 Al2 F24 Li6 O30 P12), 0.14(C4 H10 O)'
_chemical_formula_sum            'C12.55 H31.38 Al F12 Li3 O15.14 P6'
_chemical_formula_weight         886.21
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/cc13pjnz
_audit_creation_date             2014-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-11-11 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.4058(4)
_cell_length_b                   17.4058(4)
_cell_length_c                   21.4947(6)
_cell_measurement_reflns_used    6176
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.735
_cell_measurement_theta_min      2.340
_cell_volume                     5639.6(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22369
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.011
_diffrn_reflns_theta_min         2.843
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1247 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.8926. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       block
_exptl_crystal_F_000             2687
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3662
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0358P)^2^+7.2552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2953
_reflns_number_total             3662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00469a2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7034458--7034459.cif.'
_cod_original_cell_volume        5639.6(3)
_cod_database_code               7034458
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Others
 Fixed Sof: C1C(0.046) H1CA(0.046) H1CB(0.046) H1CC(0.046) C2C(0.046)
 H2CA(0.046) H2CB(0.046) O3C(0.046) C4C(0.046) H4CA(0.046) H4CB(0.046)
 C5C(0.046) H5CA(0.046) H5CB(0.046) H5CC(0.046)
 Fixed U13: Al1(0)
 Fixed U23: Al1(0)
 Fixed Uiso: H1A(0.053) H1B(0.053) H2A(0.084) H2B(0.084) H2C(0.084) H3A(0.046)
 H3B(0.046) H4A(0.068) H4B(0.068) H4C(0.068) C1C(0.05) H1CA(0.075) H1CB(0.075)
 H1CC(0.075) C2C(0.05) H2CA(0.06) H2CB(0.06) O3C(0.05) C4C(0.05) H4CA(0.06)
 H4CB(0.06) C5C(0.05) H5CA(0.075) H5CB(0.075) H5CC(0.075)
 Fixed X: Al1(0.3333) H1A(0.7665) H1B(0.7249) H2A(0.6661) H2B(0.7075)
 H2C(0.6108) H3A(0.6966) H3B(0.5985) H4A(0.591) H4B(0.5447) H4C(0.6424)
 H1CA(0.3004) H1CB(0.2908) H1CC(0.3852) H2CA(0.2367) H2CB(0.3318) H4CA(0.3361)
 H4CB(0.2535) H5CA(0.3665) H5CB(0.4339) H5CC(0.3521)
 Fixed Y: Al1(0.6667) H1A(0.7141) H1B(0.727) H2A(0.5653) H2B(0.5887)
 H2C(0.5748) H3A(0.6937) H3B(0.617) H4A(0.7035) H4B(0.7145) H4C(0.7906)
 H1CA(0.6322) H1CB(0.7062) H1CC(0.7118) H2CA(0.5778) H2CB(0.5835) H4CA(0.5814)
 H4CB(0.5941) H5CA(0.6596) H5CB(0.7208) H5CC(0.7334)
 Fixed Z: H1A(0.415) H1B(0.3523) H2A(0.4166) H2B(0.3481) H2C(0.3607)
 H3A(0.5088) H3B(0.4904) H4A(0.5709) H4B(0.5099) H4C(0.5288) H1CA(0.5197)
 H1CB(0.5574) H1CC(0.5528) H2CA(0.6168) H2CB(0.6121) H4CA(0.7063) H4CB(0.7257)
 H5CA(0.8004) H5CB(0.7473) H5CC(0.7665)
;
_shelx_res_checksum              35428
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'