Half-Sandwich Group 8 Borylene Complexes: Synthetic and Structural Studies and Oxygen Atom Abstraction Chemistry
Pierce, Glesni A.; Vidovic, Dragoslav; Kays, Deborah L.; Coombs, Natalie D.; Thompson, Amber L.; Jemmis, Eluvathingal D.; De, Susmita; Aldridge, Simon; Organometallics 28 (2009) 2947–; doi:10.1021/om801215b

data_4069042
_publ_section_title
;
 Half-Sandwich Group 8 Borylene Complexes: Synthetic and Structural
 Studies and Oxygen Atom Abstraction Chemistry
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2947
_journal_paper_doi               10.1021/om801215b
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C21 H36 B1 Cl1 Fe1 N1 O1 P1, 0.5(C5 H12)'
_chemical_formula_sum            'C23.5 H42 B Cl Fe N O P'
_chemical_formula_weight         487.68
_chemical_melting_point          ?
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-02-13
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 93.8710(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.75620(10)
_cell_length_b                   12.30200(10)
_cell_length_c                   15.96190(10)
_cell_measurement_reflns_used    6399
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2695.05(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51592
_diffrn_reflns_theta_full        26.952
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         5.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_yellow
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9653
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         6134
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.001908
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.36P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1123
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1123
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4993
_reflns_number_total             6134
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.57
_oxford_diffrn_Wilson_scale      6.62
_oxford_refine_ls_r_factor_ref   0.0541
_oxford_refine_ls_scale          0.3942(5)
_oxford_reflns_number_all        6134
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 710
_cod_data_source_file            om801215b_si_001.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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 1715 2011-07-08 13:25:40Z adriana 

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      'P 1 21/n 1 '
_cod_original_formula_sum        'C23.50 H42 B1 Cl1 Fe1 N1 O1 P1'
_cod_database_code               4069042