Syntheses and solid-state structures of [{K(THF)2(PHTipp)K(THF)(μ-THF)(PHTipp)}x]2 and [Rb(THF)(PHTipp)]x (Tipp = 2,4,6-Pri3C6H2)
Christoph Frenzel; Fernando Somoza Jr.; Steffen Blaurock; Evamarie Hey-Hawkins; J. Chem. Soc., Dalton Trans.  (2001) 3115–3118; doi:10.1039/b104576h

data_7010861
_publ_section_title
;
 Syntheses and solid-state structures of
 [{K(THF)2(PHTipp)K(THF)(\m-THF)(PHTipp)}x]2 and [Rb(THF)(PHTipp)]x
 (Tipp = 2,4,6-Pri3C6H2)
;
_journal_issue                   20
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3115
_journal_page_last               3118
_journal_paper_doi               10.1039/b104576h
_journal_year                    2001
_chemical_formula_sum            'C46 H80 K2 O4 P2'
_chemical_formula_weight         837.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.202(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.9726(10)
_cell_length_b                   11.5969(3)
_cell_length_c                   28.4498(9)
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      1.56
_cell_volume                     10440.2(5)
_computing_cell_refinement       'SAINT (AXS-Bruker)'
_computing_data_collection       'SMART (AXS-Bruker)'
_computing_data_reduction        'SAINT (AXS-Bruker)'
_computing_molecular_graphics    'XP (AXS-Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'CCD-Diffractometer (AXS-Bruker)'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20635
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.9465
_exptl_absorpt_correction_T_min  0.8969
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8443
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0825
_refine_ls_shift/su_max          0.270
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0000P)^2^+32.1969P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                5549
_reflns_number_total             8443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104576h.txt
_cod_data_source_block           c268
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010861