Low-coordinate cobalt(II) terphenyl complexes: precursors to sterically encumbered ketones
Benjamin M. Gridley; Alexander J. Blake; Adrienne L. Davis; William Lewis; Graeme J. Moxey; Deborah L. Kays; Chem.Commun. 48 (2012) 8910–; doi:10.1039/c2cc34525k

data_7108246
_publ_section_title
;
 Low-coordinate cobalt(II) terphenyl complexes: precursors to sterically
 encumbered ketones
;
_journal_name_full               Chem.Commun.
_journal_page_first              8910
_journal_paper_doi               10.1039/c2cc34525k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C53 H34 O, 2(C4 H10 O)'
_chemical_formula_sum            'C61 H54 O3'
_chemical_formula_weight         835.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 104.637(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.933(3)
_cell_length_b                   18.322(4)
_cell_length_c                   19.888(4)
_cell_measurement_reflns_used    4594
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.22
_cell_volume                     4912.2(18)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.093
_diffrn_reflns_av_sigmaI/netI    0.102
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22879
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.35
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8569
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.12
_refine_ls_R_factor_all          0.168
_refine_ls_R_factor_gt           0.107
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.101P)^2^+5.496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.240
_refine_ls_wR_factor_ref         0.273
_reflns_number_gt                5115
_reflns_number_total             8569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34525k.txt
_cod_data_source_block           2
_cod_original_cell_volume        4912.4(17)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7108246
_nottingham_internal_coll_name   COBG2D
_nottingham_internal_coll_number 10281
_nottingham_internal_coll_client BG/DLK
_nottingham_internal_coll_type   hemi
_nottingham_internal_coll_frame_time '40 s'
_nottingham_internal_coll_frame_width '0.3 degrees'
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   BMG
_nottingham_internal_coll_date   13/04/11
_nottingham_internal_process_user BMG
_nottingham_internal_process_date 14/04/2011
_nottingham_internal_solution_user BMG
_nottingham_internal_solution_date 14/04/2011
_nottingham_internal_refinement_user BMG
_nottingham_internal_refinement_date 05/10/2011