Syntheses, Structures, and Properties of Substituted Co(C5Me5)(2,7-di(OCH3)fluorenido Co(II) and Co(III) Complexes
Bugenhagen, Bernhard E. C.; Brinn, Lisa; Prosenc, Marc H.; Organometallics 33 (2014) 7015–; doi:10.1021/om500928w

data_4085023
_publ_section_title
;
 Syntheses, Structures, and Properties of Substituted
 Co(C5Me5)(2,7-di(OCH3)fluorenido Co(II) and Co(III) Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7015
_journal_paper_doi               10.1021/om500928w
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C25 H28 Co O2, B F4'
_chemical_formula_sum            'C25 H28 B Co F4 O2'
_chemical_formula_weight         506.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_cell_angle_alpha                90
_cell_angle_beta                 103.727(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8337(2)
_cell_length_b                   19.9117(5)
_cell_length_c                   11.9202(3)
_cell_measurement_reflns_used    5478
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      35.5807
_cell_measurement_theta_min      6.8547
_cell_volume                     2267.38(9)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 10.4127
_diffrn_measured_fraction_theta_full 0.9852
_diffrn_measured_fraction_theta_max 0.9852
_diffrn_measurement_details
;
  1 omega -130.00  -44.00   1.0000  140.7900
omega____ theta____ kappa____ phi______ frames
    -      -52.4271  -57.0000  150.0000 86

  2 omega    4.00   96.00   1.0000  140.7900
omega____ theta____ kappa____ phi______ frames
    -       52.5834 -125.0000  -90.0000 92

  3 omega   27.00  124.00   1.0000  140.7900
omega____ theta____ kappa____ phi______ frames
    -       52.5834   57.0000    0.0000 97
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0273546000
_diffrn_orient_matrix_UB_12      -0.0183793000
_diffrn_orient_matrix_UB_13      -0.0406604000
_diffrn_orient_matrix_UB_21      -0.0293593000
_diffrn_orient_matrix_UB_22      0.0237306000
_diffrn_orient_matrix_UB_23      -0.0433763000
_diffrn_orient_matrix_UB_31      0.0624802000
_diffrn_orient_matrix_UB_32      0.0191899000
_diffrn_orient_matrix_UB_33      0.0147083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20037
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.000
_diffrn_reflns_theta_min         3.0
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method 'From dichloromethane / hexane'
_exptl_crystal_size_max          0.2545
_exptl_crystal_size_mid          0.1583
_exptl_crystal_size_min          0.0602
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         9829
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0647P)^2^+1.8580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6849
_reflns_number_total             9829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500928w_si_001.cif
_cod_data_source_block           bb251
_cod_depositor_comments
'Adding full bibliography for 4085022--4085023.cif.'
_cod_original_cell_volume        2267.37(9)
_cod_database_code               4085023
_chemical_oxdiff_formula         'C25 H30 B1 Co1 F4 O2'
_chemical_oxdiff_usercomment     'bugenhagen / prosenc / .2 .2 .1 / plate'
_shelxl_version_number           2013-3