Coordination chemistry of a bulky redox-active cyanomanganese carbonyl ligand: N-bound tetrahedral complexes of 3d metals
Connelly, Neil G.; Hicks, Owen M.; Lewis, Gareth R.; Orpen, A. Guy; Wood, Andrew J.; Journal of the Chemical Society, Dalton Transactions  (2000) 1637–; doi:10.1039/b001782p

data_7009540
_publ_section_title
;
 Coordination chemistry of a bulky redox-active cyanomanganese carbonyl
 ligand: N-bound tetrahedral complexes of 3d metals
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1637
_journal_paper_doi               10.1039/b001782p
_journal_year                    2000
_chemical_formula_sum            'C53 H46 Cl5 Mn2 N O P4'
_chemical_formula_weight         1124.0
_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                 104.31(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.629(3)
_cell_length_b                   23.525(4)
_cell_length_c                   18.306(4)
_cell_measurement_reflns_used    219
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.00
_cell_measurement_theta_min      1.73
_cell_volume                     5270(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25042
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plates
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         8215
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_obs          0.0521
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+8.1546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1416
_refine_ls_wR_factor_obs         0.1193
_reflns_number_observed          5433
_reflns_number_total             8253
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001782p.txt
_cod_data_source_block           13.CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+8.1546P] 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^)+(0.0615P)^2^+8.1546P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5270.0(18)
_cod_original_sg_symbol_H-M      'P 1 2(1)/c 1'
_cod_database_code               7009540