Crystal structure of (18-crown-6)potassium(I) [(1,2,3,4,5-η)-cycloheptadienyl][(1,2,3-η)-cycloheptatrienyl]cobalt(I)
Brennessel, William W.; Ellis, John E.; Acta Crystallographica Section E 71 (2015) 291–295; doi:10.1107/S2056989015003151

data_2240448
_publ_section_title
;
 Crystal structure of (18-crown-6)potassium(I)
 [(1,2,3,4,5-\h)-cycloheptadienyl][(1,2,3-\h)-cycloheptatrienyl]cobalt(I)
;
_journal_coeditor_code           BH2504
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              291
_journal_page_last               295
_journal_paper_doi               10.1107/S2056989015003151
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[K (C12 H24 O6)] [Co (C7 H7) (C7 H9)]'
_chemical_formula_moiety         'C14 H16 Co, C12 H24 K O6'
_chemical_formula_sum            'C26 H40 Co K O6'
_chemical_formula_weight         546.61
_chemical_name_common            4301
_chemical_name_systematic
;
(18-Crown-6)potassium(I)
[(1,2,3,4,5-\h)-cycloheptadienyl][(1,2,3-\h)-cycloheptatrienyl]cobalt(I)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.6077(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3925(19)
_cell_length_b                   17.225(2)
_cell_length_c                   18.678(2)
_cell_measurement_reflns_used    3984
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.37
_cell_volume                     5271.9(10)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2015)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens SMART CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            85092
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         1.243
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2012)
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.472
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         12058
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+2.3296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                9117
_reflns_number_total             12058
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2504sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        5271.8(11)
_cod_database_code               2240448
_cod_database_fobs_code          2240448
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.876
_shelx_hkl_checksum              44676
_shelx_res_checksum              89255