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_7212644
_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_absolute_configuration ad
_chemical_formula_moiety         'C30 H20 Cl2 Co N6, 3(F6 P), C2 H3 N'
_chemical_formula_sum            'C32 H23 Cl2 Co F18 N7 P3'
_chemical_formula_weight         1070.31
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-01-15
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3767(6)
_cell_length_b                   12.2742(4)
_cell_length_c                   19.5992(7)
_cell_measurement_reflns_used    9070
_cell_measurement_temperature    173
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3939.7(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            134907
_diffrn_reflns_theta_full        30.087
_diffrn_reflns_theta_max         30.087
_diffrn_reflns_theta_min         1.958
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.80
_refine_ls_abs_structure_details 'Flack (1983), 5604 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.012(7)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         9981
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001751
_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:
0.525 0.322 0.271
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0390
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0356
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                10444
_reflns_number_total             11536
_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   0.0301
_oxford_refine_ls_scale          0.3132(3)
_oxford_reflns_number_all        11471
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'kh262_173k_0ma in Pna2(1)'
_cod_data_source_file            c002834g.txt
_cod_data_source_block           kh262
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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        'C32 H23 Cl2 Co1 F18 N7 P3'
_cod_database_code               7212644