Arrested B‒H Activation en Route to Installation of a PBP Pincer Ligand on Ruthenium and Osmium
Hill, Anthony F.; McQueen, Caitlin M. A.; Organometallics 33 (2014) 1977–; doi:10.1021/om5001106

data_4082966
_publ_section_title
;
 Arrested B--H Activation en Route to Installation of a PBP Pincer Ligand
 on Ruthenium and Osmium
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1977
_journal_paper_doi               10.1021/om5001106
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C50 H44 B1 Cl2 N2 Os1 P3, 0.5(C7 H8)'
_chemical_formula_sum            'C53.5 H48 B Cl2 N2 Os P3'
_chemical_formula_weight         1083.82
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 92.0176(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.42330(10)
_cell_length_b                   20.3953(2)
_cell_length_c                   18.8159(2)
_cell_measurement_reflns_used    72954
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     4764.56(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows v. 2.01'
_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      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_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  0.036
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            102412
_diffrn_reflns_theta_full        27.484
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.585
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.928
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.91
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10912
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.0103199
_refine_ls_shift/su_mean         0.0003594
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 4.18P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0538
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0538
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                9626
_reflns_number_total             10913
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.68
_oxford_diffrn_Wilson_scale      43.31
_oxford_refine_ls_r_factor_ref   0.0272
_oxford_refine_ls_scale          0.18853(4)
_oxford_reflns_number_all        10912
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om5001106_si_001.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4082965--4082967.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C53.50 H48 B1 Cl2 N2 Os1 P3'
_cod_database_code               4082966
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, OS(1,U'S) UNTIL C(87) 
REM CONT C(81,U[ISO]) UNTIL C(87) 
CONT H(1, X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) H   ( 872,X'S) H   ( 873,X'S) 
CONT H   ( 881,X'S) H   ( 882,X'S) H   ( 883,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
U(IJ) 0.0, 0.01 = C(81) TO C(82) 
U(IJ) 0.0, 0.01 = C(82) TO C(83) 
U(IJ) 0.0, 0.01 = C(83) TO C(84) 
U(IJ) 0.0, 0.01 = C(84) TO C(85) 
U(IJ) 0.0, 0.01 = C(85) TO C(86) 
U(IJ) 0.0, 0.01 = C(86) TO C(81) 
U(IJ) 0.0, 0.01 = C(87) TO C(81) 
DIST 1.39, 0.01 = C(81) TO C(82), C(82) TO C(83), C(83) TO C(84) 
DIST 1.39, 0.01 = C(84) TO C(85), C(85) TO C(86), C(86) TO C(81) 
DIST 1.5, 0.02 = C(81) TO C(87) 
ANGLE 120, 0.1 = C(81) TO C(82) TO C(83), C(82) TO C(83) TO C(84) 
ANGLE 120, 0.1 = C(83) TO C(84) TO C(85), C(84) TO C(85) TO C(86) 
ANGLE 120, 0.1 = C(85) TO C(86) TO C(81), C(86) TO C(81) TO C(82) 
ANGLE 120, 0.1 = C(86) TO C(81) TO C(87), C(82) TO C(81) TO C(87) 
LIMIT 0.001 FOR C(82,X) 
END                                                                             
;