Easy Access to Hydride Chemistry on a Tripodal P-Based Rhodium Scaffold
Tejel, Cristina; Geer, Ana M.; Jiménez, Sonia; López, José A.; Ciriano, Miguel A.; Organometallics 31 (2012) 2895–; doi:10.1021/om201129j

data_4077961
_publ_section_title
;
 Easy Access to Hydride Chemistry on a Tripodal P-Based Rhodium Scaffold
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2895
_journal_paper_doi               10.1021/om201129j
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C51 H50 B N3 P3 Rh, 3(C6 D6), 2(B  F4)'
_chemical_formula_sum            'C69 H50 B3 D18 F8 N3 P3 Rh'
_chemical_formula_weight         1337.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.6362(10)
_cell_angle_beta                 76.7235(10)
_cell_angle_gamma                79.7700(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9713(10)
_cell_length_b                   13.0463(10)
_cell_length_c                   19.7923(15)
_cell_measurement_reflns_used    7657
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      2.40
_cell_volume                     3182.0(4)
_computing_cell_refinement       'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 4.0 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_computing_molecular_graphics
;
ORTEP3 for Windows - L. J. Farrugia, 
J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_structure_refinement
;
SHELX97 - Programs for Crystal Structure Analysis (Release 97-2). 
G. M. Sheldrick, Institut fur Anorganische Chemie der Universitat, 
Tammanstrasse 4, D-3400 Gottingen, Germany, 1998.
;
_computing_structure_solution
;
SHELX97 - Programs for Crystal Structure Analysis (Release 97-2). 
G. M. Sheldrick, Institut fur Anorganische Chemie der Universitat, 
Tammanstrasse 4, D-3400 Gottingen, Germany, 1998.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37706
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.9435
_exptl_absorpt_correction_T_min  0.8343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2008/1: Area-Detector Absorption Correction. Bruker-AXS 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         13826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+2.2541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                10289
_reflns_number_total             13826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201129j_si_002.cif
_cod_data_source_block           ctb76as
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               4077961