Bulk Synthesis of Octa- and Nonamethylfluorene (Flu‘ ‘H and Flu*H) and the Characterization of the Organometallic Derivatives Flu*SnMe3, [(FeCp)2Flu*H][PF6]2, and [(FeCp)2Flu‘ ‘H][PF6]2
Moss, James; Thomas, Jemima; Ashley, Andrew; Cowley, Andrew R.; O'Hare, Dermot; Organometallics 25 (2006) 4279–; doi:10.1021/om0603666

data_4075555
_publ_section_title
;
 Bulk Synthesis of Octa- and Nonamethylfluorene
 (Flu&#x2018;&#x00A0;&#x2018;H and Flu*H) and the Characterization of the
 Organometallic Derivatives Flu*SnMe3, [(FeCp)2Flu*H][PF6]2, and
 [(FeCp)2Flu&#x2018;&#x00A0;&#x2018;H][PF6]2
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4279
_journal_paper_doi               10.1021/om0603666
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C31 H36 Fe2, 2( F6 P ) '
_chemical_formula_sum            'C31 H36 F12 Fe2 P2'
_chemical_formula_weight         810.24
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.2940(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3125(3)
_cell_length_b                   17.3087(5)
_cell_length_c                   6.7634(2)
_cell_measurement_reflns_used    8457
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1542.14(7)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
; 
Nonius KappaCCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8457
_diffrn_reflns_theta_full        27.486
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         5.209
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_thermal_history
; 
The material was crystallised at ambient temperature. A suitable crystal 
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. 
;
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0821
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         1505
_refine_ls_number_restraints     167
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.012007
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.743 0.428 0.432 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0648
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0585
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                1505
_reflns_number_total             1814
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            om0603666si20060427_115634.cif
_cod_data_source_block           arc1483
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_refinement_disorder_assembly' tag replaced with
'_atom_site_disorder_assembly'.

'_atom_site_refinement_disorder_group'
tag replaced with '_atom_site_disorder_group'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 1 2/m 1 '
_cod_original_formula_sum        ' C31 H36 F12 Fe2 P2 '
_cod_database_code               4075555