Hydrogen Bonding of CHCl3 to Coordinated Nitric Oxide in a Binuclear Metallomacrocycle and the Crystal Structures of anti-[Mo(NO){HB(3,5-Me2C3HN2)3}(2,7-O2C10H6)]2.2CHCl3.CH2Cl2, syn-[Mo(NO){HB(3,5-Me2C3HN2)3}(2,7-O2C10H6)]2.0.67CHCl3.2.7H2O, and syn-[Mo(NO){HB(3,5-Me2C3HN2)3}(2,7-O2C10H6)]2.3(CH3)2CO
Ferida S. McQuillan; Hongli Chen; Thomas A. Hamor; Christopher J. Jones; Keith Paxton; Inorganic Chemistry 36 (1997) 4458–4464; doi:10.1021/ic9706820

data_4323609
_publ_section_title
;
 Hydrogen Bonding of CHCl3 to Coordinated Nitric Oxide in a Binuclear
 Metallomacrocycle and the Crystal Structures of
 anti-[Mo(NO){HB(3,5-Me2C3HN2)3}(2,7-O2C10H6)]2.2CHCl3.CH2Cl2,
 syn-[Mo(NO){HB(3,5-Me2C3HN2)3}(2,7-O2C10H6)]2.0.67CHCl3.2.7H2O, and
 syn-[Mo(NO){HB(3,5-Me2C3HN2)3}(2,7-O2C10H6)]2.3(CH3)2CO
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4458
_journal_page_last               4464
_journal_paper_doi               10.1021/ic9706820
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C50.67 H62.08 B2 Cl2 Mo2 N14 O8.71'
_chemical_formula_weight         1290.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 99.86(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.770(7)
_cell_length_b                   26.600(10)
_cell_length_c                   11.334(4)
_cell_measurement_temperature    293(2)
_cell_volume                     7060(4)
_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         'rotating anode'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9035
_diffrn_reflns_theta_max         23.55
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.484
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             2647
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         9035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_obs          0.0692
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1634P)^2^+4.2400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2439
_refine_ls_wR_factor_obs         0.2334
_reflns_number_observed          7598
_reflns_number_total             9035
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9706820_2.cif
_cod_data_source_block           structure_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1634P)^2^+4.2400P] 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^)+( 0.1634P)^2^+4.2400P] 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        7060.4(42)
_cod_database_code               4323609