A new polymorph of tetraethylammonium tris(μ-acetato-<i>O,O</i>')tri-μ-chloro-trichloro-μ~3~-oxo-<i>triangulo</i>-trimolybdenum
Yu-Biao Chen; Zhao-Ji Li; Ye-Yan Qin; Yao Kang; Jian-Kai Cheng; Rui-Feng Hu; Yi-Hang Wen; Yuan-Gen Yao; Acta Crystallographica Section E 58 (2002) m490–m491; doi:10.1107/S1600536802013892

data_2201287
_publ_section_title
;A new polymorph of tetraethylammonium
 tris(\m-acetato-<i>O,O</i>')tri-\m-chloro-trichloro-\m~3~-oxo-<i>triangulo</i>-trimolybdenum
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m490
_journal_page_last               m491
_journal_paper_doi               10.1107/S1600536802013892
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C2 H5 N) [Mo3 Cl6 O (C2 H3 O2)3]'
_chemical_formula_moiety         'C14 H29 Cl6 Mo3 N O7'
_chemical_formula_sum            'C14 H29 Cl6 Mo3 N O7'
_chemical_formula_weight         823.90
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.6130(10)
_cell_angle_beta                 92.5180(10)
_cell_angle_gamma                91.8150(10)
_cell_formula_units_Z            4
_cell_length_a                   7.93560(10)
_cell_length_b                   14.42580(10)
_cell_length_c                   24.4415(4)
_cell_measurement_reflns_used    6220
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      .84
_cell_volume                     2774.80(6)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'XPREP (Sheldrick, 1991)'
_computing_molecular_graphics    'XP (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14579
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         0.84
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          .84
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .02
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.805
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+55.1956P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1574
_reflns_number_gt                7292
_reflns_number_total             9771
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6175.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2201287
_cod_database_fobs_code          2201287