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_4085022
_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'
_chemical_formula_sum            'C25 H28 Co O2'
_chemical_formula_weight         419.40
_chemical_name_systematic
2,7-dimethoxyfluorenyl-pentamethylcyclopentadienylcobalt(II)
_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     direct
_audit_update_record
;
2013-09-14 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 104.244(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5015(3)
_cell_length_b                   8.31079(16)
_cell_length_c                   19.7907(5)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.1290
_cell_measurement_theta_min      3.3990
_cell_volume                     1992.99(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.4127
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9271
_diffrn_measurement_details
;
  1 omega    1.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3895   38.0000  -60.0000 93

  2 omega  -16.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3895   38.0000 -150.0000 110

  3 omega  -64.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3895  -57.0000  150.0000 111

  4 omega   39.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3895 -178.0000  150.0000 66

  5 omega  -20.00   58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3895  -99.0000  -60.0000 78

  6 omega  -21.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3895   77.0000   60.0000 117
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0574475000
_diffrn_orient_matrix_UB_12      0.0009824000
_diffrn_orient_matrix_UB_13      -0.0020726000
_diffrn_orient_matrix_UB_21      0.0088767000
_diffrn_orient_matrix_UB_22      0.0561786000
_diffrn_orient_matrix_UB_23      0.0278079000
_diffrn_orient_matrix_UB_31      -0.0068787000
_diffrn_orient_matrix_UB_32      0.0642362000
_diffrn_orient_matrix_UB_33      -0.0242914000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description
;
;
_exptl_crystal_F_000             884
_exptl_crystal_preparation
'At room-temperature, a solution of Co(II)Cp*acac in THF was treated with an equimolar quantity of Sodium-(2,7-dimethoxyfluorenide) whereupon the Solution turned green. After stirring overnight, the solvent was removed in vacuo, the reaction mixture suspended in hexane and filtered over glass-wool. A green, amorphous, extremely air and moisture sensitive powder was obtained (41 mg, XX% yield)'
_exptl_crystal_recrystallization_method
'Single-crystals suitable for x-ray diffraction were obtained from a solution in n-hexane by evaporation'
_exptl_crystal_size_max          0.2422
_exptl_crystal_size_mid          0.2048
_exptl_crystal_size_min          0.1529
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0462P)^2^+1.5324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3686
_reflns_number_total             4566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500928w_si_001.cif
_cod_data_source_block           bb_lb6
_cod_depositor_comments
'Adding full bibliography for 4085022--4085023.cif.'
_cod_database_code               4085022
_shelxl_version_number           2013-4