Syntheses of Metallomacrocycles Containing Metal Amide Linkages. The X-ray Crystal Structure of syn-[{Mo(NO)[HB(3,5- Me2C3HN2)3]}{(4-NHC6H4)2CO}]2
Helen A. Jones; Thomas A. Hamor; Christopher J. Jones; Ferida S. McQuillan; Keith Paxton; Natalie M. Rowley; Inorganic Chemistry 40 (2001) 1052–1056; doi:10.1021/ic000749a

data_4319301
_publ_section_title
;
 Syntheses of Metallomacrocycles Containing Metal Amide Linkages. The
 X-ray Crystal Structure of syn-[{Mo(NO)[HB(3,5-
 Me2C3HN2)3]}{(4-NHC6H4)2CO}]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1052
_journal_page_last               1056
_journal_paper_doi               10.1021/ic000749a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C56.5 H75 B2 Cl Mo2 N18 O9'
_chemical_formula_weight         1399.29
_chemical_name_systematic
;
?
;
_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           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.45(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.075(2)
_cell_length_b                   21.067(3)
_cell_length_c                   21.429(3)
_cell_measurement_temperature    294(2)
_cell_volume                     7643.3(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    TeXsan
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Rigaku R-axis II area detector'
_diffrn_measurement_method       'image-plate scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29125
_diffrn_reflns_theta_max         22.01
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.420
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_F_000             2892
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.137
_refine_ls_goodness_of_fit_obs   1.174
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         9137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.174
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_obs          0.0649
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1262P)^2^+4.1088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2051
_refine_ls_wR_factor_obs         0.1926
_reflns_number_observed          7630
_reflns_number_total             9137
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000749a.cif
_cod_data_source_block           jones25ccrn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1262P)^2^+4.1088P] 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^)+( 0.1262P)^2^+4.1088P] 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        7643.3(16)
_cod_original_formula_sum        'C56.50 H75 B2 Cl Mo2 N18 O9'
_cod_database_code               4319301