The [Cl2OMo(μ-OC2H5)2(μ-HOC2H5)MoOCl2]/PMe3 System: A Chameleon Yielding the X-ray Structures of MoOCl2(PMe3)3, MoOCl3(PMe3)2, Mo4O4Cl4(μ2-OEt)4(PMe3)2(μ3-O)2, and MoOCl3(OPMe3)(PMe3)
Christian Limberg; Michael Büchner; Katja Heinze; Olaf Walter; Inorganic Chemistry 36 (1997) 872–879; doi:10.1021/ic961046p

data_4323325
_publ_section_title
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 The [Cl2OMo(\m-OC2H5)2(\m-HOC2H5)MoOCl2]/PMe3 System: A Chameleon
 Yielding the X-ray Structures of MoOCl2(PMe3)3, MoOCl3(PMe3)2,
 Mo4O4Cl4(\m2-OEt)4(PMe3)2(\m3-O)2, and MoOCl3(OPMe3)(PMe3)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              872
_journal_page_last               879
_journal_paper_doi               10.1021/ic961046p
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C6 H18 Cl3 Mo O2 P2'
_chemical_formula_weight         386.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.783(3)
_cell_length_b                   12.623(4)
_cell_length_c                   18.298(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1549.2(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2362
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.549
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.847
_refine_ls_goodness_of_fit_obs   0.829
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      0.829
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_obs          0.0369
_refine_ls_shift/esd_max         -0.033
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1432
_refine_ls_wR_factor_obs         0.1043
_reflns_number_observed          1739
_reflns_number_total             2154
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961046p_4.cif
_cod_data_source_block           lido
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21 1'
_cod_database_code               4323325