The syntheses of metallomacrocycles containing unsymmetrical bridging ligands and the crystal structures of DL-[Mo{HB(3,5-Me2C3HN2)3}(NO)(OC6H4CH2CH2O-4)]2·2CH2Cl2 and DL-[W{HB(3,5-Me2C3HN2)3}(NO)(OC6H3NO2-4-CH2CH2O-3)]2· CH2Cl2 †
Berridge, Timothy E.; Barton, Matthew T.; Hamor, Thomas A.; Jones, Christopher J.; McQuillan, Ferida S.; Paxton, Keith; Rowley, Natalie M.; Journal of the Chemical Society, Dalton Transactions  (2000) 4645–; doi:10.1039/b006716o

data_7010188
_publ_section_title
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 The syntheses of metallomacrocycles containing unsymmetrical bridging
 ligands and the crystal structures of
 DL-[Mo{HB(3,5-Me2C3HN2)3}(NO)(OC6H4CH2CH2O-4)]2&#x00B7;2CH2Cl2 and
 DL-[W{HB(3,5-Me2C3HN2)3}(NO)(OC6H3NO2-4-CH2CH2O-3)]2&#x00B7;
 CH2Cl2&#x200A;&#x2020;
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4645
_journal_paper_doi               10.1039/b006716o
_journal_year                    2000
_chemical_formula_sum            'C48 H64 B2 Cl4 Mo2 N14 O6'
_chemical_formula_weight         1288.43
_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                 106.55(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.730(3)
_cell_length_b                   17.167(3)
_cell_length_c                   24.701(5)
_cell_measurement_reflns_used    21958
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.02
_cell_measurement_theta_min      1.44
_cell_volume                     5987(2)
_computing_cell_refinement       'R-Axis II software'
_computing_data_collection       'R-Axis II software'
_computing_data_reduction        TeXsan
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  SHELXL-93
_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     0.7107
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21958
_diffrn_reflns_theta_max         22.02
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.654
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         7102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0814P)^2^+1.7498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1386
_refine_ls_wR_factor_ref         0.1507
_reflns_number_observed          5763
_reflns_number_total             7102
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006716o.txt
_cod_data_source_block           tim725rn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0814P)^2^+1.7498P] 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^)+( 0.0814P)^2^+1.7498P] 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        5987.4(20)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7010188