Exploiting theo-Quinodimethane Nature of Naphthalene: Cycloaddition Reactions with η2-Coordinated Tungsten‒Naphthalene Complexes
Strausberg, Laura; Li, Mengxun; Harrison, Daniel P.; Myers, William H.; Sabat, Michal; Harman, W. Dean; Organometallics 32 (2013) 915–; doi:10.1021/om301238q

data_4080054
_publ_section_title
;
 Exploiting theo-Quinodimethane Nature of Naphthalene: Cycloaddition
 Reactions with \h2-Coordinated Tungsten--Naphthalene Complexes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              915
_journal_paper_doi               10.1021/om301238q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C29.5 H37 B Cl N8 O3 P W'
_chemical_formula_weight         812.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.142(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.7214(5)
_cell_length_b                   14.3863(2)
_cell_length_c                   13.6580(2)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      34.92
_cell_measurement_theta_min      2.49
_cell_volume                     6429.35(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30369
_diffrn_reflns_theta_full        36.26
_diffrn_reflns_theta_max         36.26
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    3.772
_exptl_absorpt_correction_T_max  0.5192
_exptl_absorpt_correction_T_min  0.3069
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.121
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         10120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                9060
_reflns_number_total             15387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301238q_si_002.cif
_cod_data_source_block           C29.5H37BClN8O3PW
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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      C2/c
_cod_original_formula_sum        'C29.50 H37 B Cl N8 O3 P W'
_cod_database_code               4080054