Ruthenium Hydrides Containing the Superhindered Polydentate Polyphosphine Ligand P(CH2CH2P(t)Bu2)3.
Gilbert-Wilson, Ryan; Field, Leslie D.; Bhadbhade, Mohan; Inorganic chemistry  (2014) 141112150820006–; doi:10.1021/ic501895s

data_4341644
_publ_section_title
;
 Ruthenium Hydrides Containing the Superhindered Polydentate Polyphosphine
 Ligand P(CH2CH2P(t)Bu2)3.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141112150820006
_journal_paper_doi               10.1021/ic501895s
_journal_year                    2014
_chemical_formula_sum            'C30 H71 B P4 Ru'
_chemical_formula_weight         667.63
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.760(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2066(3)
_cell_length_b                   22.2411(10)
_cell_length_c                   20.3594(11)
_cell_measurement_reflns_used    2183
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.101
_cell_measurement_theta_min      2.213
_cell_volume                     3690.2(3)
_computing_cell_refinement
;
        APEX2(Bruker, 2007, Bruker AXS Inc.,Madison, USA)
;
_computing_data_collection
;
        APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA)
;
_computing_data_reduction
;
        APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA)
;
_computing_molecular_graphics    'SHELXTL-Plus. Sheldrick, G. M. (2008)'
_computing_structure_refinement  'SHELXL-97. Sheldrick, G. M. (2008)'
_computing_structure_solution    'SHELXS-97. Sheldrick, G. M. (2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Area Detector'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.1140
_diffrn_reflns_av_sigmaI/netI    0.1160
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26284
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.9000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+2.7748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1306
_reflns_number_gt                3953
_reflns_number_total             6485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501895s_si_002.cif
_cod_data_source_block           RuHBH4
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/COD-crude-data--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 2935 2014-11-11 08:27:57Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4341644