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_7212646
_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 H22 Co N6, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C34 H28 Co F12 N8 P2'
_chemical_formula_weight         897.51
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-11-17
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3479(5)
_cell_length_b                   12.3479(5)
_cell_length_c                   49.146(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    123
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     7493.3(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      123
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Kappa Apex2'
_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  0.038
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            63132
_diffrn_reflns_theta_full        29.369
_diffrn_reflns_theta_max         29.369
_diffrn_reflns_theta_min         1.649
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.65
_refine_ls_abs_structure_details 'Flack (1983), 9695 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.146(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1156
_refine_ls_number_reflns         13859
_refine_ls_number_restraints     337
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.038858
_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:
0.247 0.218 0.881E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0658
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0465
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              61
_reflns_limit_l_min              -67
_reflns_number_gt                16330
_reflns_number_total             20080
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.82
_oxford_diffrn_Wilson_scale      392.22
_oxford_refine_ls_r_factor_ref   0.0425
_oxford_refine_ls_scale          0.05519(5)
_oxford_reflns_number_all        20038
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'kh429_123k_0m in P4(3)'
_cod_data_source_file            c002834g.txt
_cod_data_source_block           kh429
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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        'C34 H28 Co1 F12 N8 P2'
_cod_database_code               7212646