Exocyclic coordination of the η3-fluorenyl, η3-cyclopenta[def]phenanthrenyl and η3-8,9-dihydrocyclopenta[def]phenanthrenyl anions: X-ray crystal structures, NMR fluxionality and theoretical studies
Maria J. Calhorda; Isabel S. Gonçalves; Brian J. Goodfellow; Eberhardt Herdtweck; Carlos C. Romão; Beatriz Royo; Luís F. Veiros; New J. Chem. 26 (2002) 1552–1558; doi:10.1039/b204418h

data_7050933
_publ_section_title
;
 Exocyclic coordination of the \h3-fluorenyl,
 \h3-cyclopenta[def]phenanthrenyl and
 \h3-8,9-dihydrocyclopenta[def]phenanthrenyl anions: X-ray crystal
 structures, NMR fluxionality and theoretical studies
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              1552
_journal_page_last               1558
_journal_paper_doi               10.1039/b204418h
_journal_volume                  26
_journal_year                    2002
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C26 H16 Mo O2'
_chemical_formula_sum            'C26 H16 Mo O2'
_chemical_formula_weight         456.33
_chemical_name_systematic
;
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.899(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7600(8)
_cell_length_b                   10.8026(10)
_cell_length_c                   17.744(2)
_cell_measurement_reflns_used    4934
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      11.3
_cell_volume                     1860.9(3)
_computing_cell_refinement       'IPDS (STOE, 1997)'
_computing_data_collection       'IPDS (STOE, 1997)'
_computing_data_reduction        'IPDS (STOE, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 1999)'
_computing_publication_material  'PLATON (Spek, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'imaging plate'
_diffrn_detector_area_resol_mean 67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'one-circle diffractometer'
_diffrn_measurement_device_type  'IPDS (STOE&CIE)'
_diffrn_measurement_method       'phi-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25644
_diffrn_reflns_theta_full        25.65
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
; 
Neither decay correction nor absorption correction
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0222
_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^)+(0.0396P)^2^+0.9290P]  where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                3175
_reflns_number_total             3481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204418h.txt
_cod_data_source_block           ROMX-3077-123
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7050933