Synthesis and characterization of cobalt(ii) complexes with tripodal polypyridine ligand bearing pivalamide groups. Selective formation of six- and seven-coordinate cobalt(ii) complexes.
Matsumoto, Jun; Suzuki, Tatsuya; Kajita, Yuji; Masuda, Hideki; Dalton transactions (Cambridge, England : 2003) 41 (2012) 4107–4117; doi:10.1039/c2dt12056a

data_7018499
_publ_section_title
;
 Synthesis and characterization of cobalt(ii) complexes with tripodal
 polypyridine ligand bearing pivalamide groups. Selective formation of
 six- and seven-coordinate cobalt(ii) complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4107
_journal_page_last               4117
_journal_paper_doi               10.1039/c2dt12056a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C34 H45 Co I2 N9 O2'
_chemical_formula_sum            'C34 H45 Co I2 N9 O2'
_chemical_formula_weight         924.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.0624(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.3245(16)
_cell_length_b                   14.4477(15)
_cell_length_c                   19.422(3)
_cell_measurement_reflns_used    10516
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     3881.4(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29741
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.075
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1844.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.870
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8878
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0446P)^2^+4.0070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                7697
_reflns_number_total             8878
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2dt12056a.txt
_cod_data_source_block           110921_CuMeCN_BPPA_I2
_cod_original_cell_volume        3881.3(8)
_cod_database_code               7018499