Diethanolaminium <i>cyclo</i>-octa-μ~2~-fluoro-hexadeca-μ~2~-trimethylacetato-κ^32^<i>O</i>:<i>O</i>'-heptachromium(III)nickel(II) ethyl acetate 0.5-solvate
Larsen, Finn K.; Muryn, Christopher A.; Overgaard, Jacob; Timco, Grigore A.; Winpenny, Richard E. P.; Acta Crystallographica Section E 61 (2005) m1525–m1527; doi:10.1107/S1600536805019562

data_2206428
_publ_section_title
;Diethanolaminium
 <i>cyclo</i>-octa-\m~2~-fluoro-hexadeca-\m~2~-trimethylacetato-\k^32^<i>O</i>:<i>O</i>'-heptachromium(III)nickel(II)
 ethyl acetate 0.5-solvate
;
_journal_coeditor_code           HB6196
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1525
_journal_page_last               m1527
_journal_paper_doi               10.1107/S1600536805019562
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'(C4 H12 N O2) [Cr7 Ni F8 (C5 H9 O2)16] , 0.5C4 H8 O2'
_chemical_formula_moiety
'C4 H12 N O2 + , C80 H144 Cr7 Ni F8 O32 - , 0.5C4 H8 O2'
_chemical_formula_sum            'C86 H160 Cr7 F8 N Ni O35'
_chemical_formula_weight         2342.85
_chemical_name_systematic
;
Diethanolaminium
cyclo-octa-\m~2~-fluoro-hexadeca-\m~2~-trimethylacetato-\k^2^O:O'-
heptachromium(III)nickel(II) ethyl acetate 0.5-solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.506(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.9892(15)
_cell_length_b                   16.6220(9)
_cell_length_c                   30.8299(19)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.96
_cell_measurement_theta_min      2.19
_cell_volume                     11994.4(12)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    SHELXL97
_computing_publication_material
;
enCIFer (Version 1.1; Allen <i>et al.</i>, 2004) and WinGX (Version
1.70.00;  Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX-II'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            209153
_diffrn_reflns_theta_full        31.13
_diffrn_reflns_theta_max         31.13
_diffrn_reflns_theta_min         2.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4908
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.103
_refine_diff_density_min         -1.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         38517
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0907
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1134P)^2^+52.1149P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2577
_reflns_number_gt                28754
_reflns_number_total             38517
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6196.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C86 H160 Cr7 Ni F8 N O35'
_cod_database_code               2206428
_cod_database_fobs_code          2206428