Crystal structure of [bis(2,6-diisopropylphenyl) phosphato-κ<i>O</i>]tris(methanol-κ<i>O</i>)lithium methanol monosolvate
Minyaev, Mikhail E.; Nifant'ev, Ilya E.; Tavtorkin, Alexander N.; Korchagina, Sof'ya A.; Zeynalova, Shadana Sh.; Acta Crystallographica Section E 71 (2015) 443–446; doi:10.1107/S2056989015005563

data_2240534
_publ_section_title
;
 Crystal structure of [bis(2,6-diisopropylphenyl)
 phosphato-\k<i>O</i>]tris(methanol-\k<i>O</i>)lithium methanol
 monosolvate
;
_journal_coeditor_code           WM5137
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              443
_journal_page_last               446
_journal_paper_doi               10.1107/S2056989015005563
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Li (C24 H34 O4 P) (C H4 O)3], C H4 O'
_chemical_formula_moiety         'C27 H46 Li O7 P, C H4 O'
_chemical_formula_sum            'C28 H50 Li O8 P'
_chemical_formula_weight         552.59
_chemical_name_systematic
;
[Bis(2,6-diisopropylphenyl)
phosphato-\k<i>O</i>]tris(methanol-\k<i>O</i>)lithium
methanol monosolvate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90.855(2)
_cell_angle_beta                 102.859(2)
_cell_angle_gamma                118.6830(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1853(6)
_cell_length_b                   11.5046(6)
_cell_length_c                   14.5237(7)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.34
_cell_measurement_theta_min      2.26
_cell_volume                     1582.21(14)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710730(9)
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.336
_diffrn_reflns_theta_min         2.039
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.8718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.527
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         10353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0628P)^2^+0.3290P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                8544
_reflns_number_total             10353
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5137sup1.cif
_cod_data_source_block           I
_cod_database_code               2240534
_cod_database_fobs_code          2240534
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              83003
_shelx_res_checksum              82274
_shelxl_version_number           2.014