An entry to half-sandwich complexes of first row transition metals (Ni, Co, Mn) containing the Kläui tripodal ligand, LOMe: synthesis and crystal structures of oligomeric, [LOMeM(μ-X)(L)]n (n = 2, 4), and monomeric complexes, LOMeM(L2)(X)
De-qiang Ma; Shiro Hikichi; Munetaka Akita; Yoshihiko Moro-oka; J. Chem. Soc., Dalton Trans.  (2000) 1123–1134; doi:10.1039/a909580b

data_7009255
_publ_section_title
;
 An entry to half-sandwich complexes of first row transition metals
 (Ni, Co, Mn) containing the Kl\"aui tripodal ligand, LOMe: synthesis
 and crystal structures of oligomeric, [LOMeM(\m-X)(L)]n
 (n&#x00A0;=&#x00A0;2, 4), and monomeric complexes, LOMeM(L2)(X)
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1123
_journal_page_last               1134
_journal_paper_doi               10.1039/a909580b
_journal_year                    2000
_chemical_formula_sum            'C21 H31 Co N5 Ni O9 P3'
_chemical_formula_weight         708.06
_chemical_name_common            'compound 10'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 109.61(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.959(7)
_cell_length_b                   11.083(4)
_cell_length_c                   19.026(3)
_cell_measurement_temperature    213(2)
_cell_volume                     2772.7(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5521
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.509
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_F_000             1456
_refine_diff_density_max         0.816
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.487
_refine_ls_goodness_of_fit_obs   1.509
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.487
_refine_ls_restrained_S_obs      1.509
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_obs          0.0624
_refine_ls_shift/esd_max         0.578
_refine_ls_shift/esd_mean        0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1737
_refine_ls_wR_factor_obs         0.1716
_reflns_number_observed          5238
_reflns_number_total             5521
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a909580b.txt
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2772.6(17)
_cod_database_code               7009255