The synthesis and structure of a paramagnetic Lewis base adduct of antimony pentachloride, trans-[MnII(CNSbCl5)(CO)2{P(OEt)3}(dppm)][SbCl6] †
Bellamy, Dena; Brown, Nathan C.; Connelly, Neil G.; Orpen, A. Guy; Journal of the Chemical Society, Dalton Transactions  (1999) 3191–; doi:10.1039/a902481f

data_7027429
_publ_section_title
;
 The synthesis and structure of a paramagnetic Lewis base adduct of
 antimony pentachloride,
 trans-[MnII(CNSbCl5)(CO)2{P(OEt)3}(dppm)][SbCl6]&#x200A;&#x2020;
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3191
_journal_paper_doi               10.1039/a902481f
_journal_year                    1999
_chemical_formula_sum            'C35 H39 Cl13 Mn N O5 P3 Sb2'
_chemical_formula_weight         1405.60
_chemical_name_systematic
; 
 ? 
;
_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                 97.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.267(3)
_cell_length_b                   13.822(3)
_cell_length_c                   24.993(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5565(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21246
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.934
_exptl_absorpt_correction_T_max  .679
_exptl_absorpt_correction_T_min  .419
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.111
_refine_ls_goodness_of_fit_obs   1.099
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         7940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_obs          0.0476
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+16.3736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1334
_refine_ls_wR_factor_obs         0.1205
_reflns_number_observed          6754
_reflns_number_total             7948
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902481Fsup1.cif
_cod_data_source_block           nabs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+16.3736P] 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^)+(0.0550P)^2^+16.3736P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2018-02-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C140 H156 Cl52 Mn4 N4 O20 P12 Sb8'
_cod_original_formula_weight         5623.49
_cod_original_formula_units_Z            1
_cod_original_cell_volume        5565.7(19)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027429