Turning {M(tpy)2}n+ embraces and CH⋯π interactions on and off in homoleptic cobalt(ii) and cobalt(iii) bis(2,2′:6′,2″-terpyridine) complexes
Constable, Edwin C.; Harris, Kate; Housecroft, Catherine E.; Neuburger, Markus; Zampese, Jennifer A.; CrystEngComm 12 (2010) 2949–; doi:10.1039/c002834g

data_7212639
_publ_section_related_literature
;
?
;
_publ_section_title
;
 Turning {M(tpy)2}n+ embraces and CH&#x22EF;\p interactions on and off in
 homoleptic cobalt(ii) and cobalt(iii)
 bis(2,2&#x2032;:6&#x2032;,2&#x2033;-terpyridine) complexes
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2949
_journal_paper_doi               10.1039/c002834g
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C36 H34 Co N6 O2, 3(F6 P), 2.5(C2 H3 N)'
_chemical_formula_sum            'C41 H41.5 Co F18 N8.5 O2 P3'
_chemical_formula_weight         1179.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-01-07
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                72.619(2)
_cell_angle_beta                 89.8082(17)
_cell_angle_gamma                78.331(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5795(4)
_cell_length_b                   13.4992(4)
_cell_length_c                   20.4174(8)
_cell_measurement_reflns_used    12113
_cell_measurement_temperature    173
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1
_cell_volume                     2720.17(17)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23232
_diffrn_reflns_theta_full        25.894
_diffrn_reflns_theta_max         27.843
_diffrn_reflns_theta_min         1.047
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1194
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         8084
_refine_ls_number_restraints     1127
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.001759
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.18 1.04 0.811
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1008
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0705
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6447
_reflns_number_total             12782
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0773
_oxford_refine_ls_scale          0.2745(5)
_oxford_reflns_number_all        12674
_oxford_reflns_threshold_expression_ref I>1.0\s(I)
_oxford_structure_analysis_title '11031336 kh082_173k'
_cod_data_source_file            c002834g.txt
_cod_data_source_block           kh082
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_formula_sum        'C41 H41.50 Co1 F18 N8.50 O2 P3'
_cod_database_code               7212639