A short and modular synthesis of bulky and electron-rich N-phosphinomethyl-functionalised N-heterocyclic carbene complexes.
Brill, Marcel; Kühnel, Erik; Scriban, Corina; Rominger, Frank; Hofmann, Peter; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12861–12864; doi:10.1039/c3dt51777b

data_7021822
_publ_section_title
;
 A short and modular synthesis of bulky and electron-rich
 N-phosphinomethyl-functionalised N-heterocyclic carbene complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12861
_journal_page_last               12864
_journal_paper_doi               10.1039/c3dt51777b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C19 H36 B F4 N2 P Pd'
_chemical_formula_weight         516.68
_chemical_name_common            'in manuscript tBu-5'
_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                 110.823(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6630(11)
_cell_length_b                   20.616(2)
_cell_length_c                   12.8353(15)
_cell_measurement_reflns_used    4581
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.29
_cell_volume                     2389.9(5)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX'
_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  0.0952
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34161
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  0.9093
_exptl_absorpt_correction_T_min  0.8505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4288
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0239P)^2^+6.4996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                3103
_reflns_number_total             4288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51777b.txt
_cod_data_source_block           mbi23
_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 
;
_cod_original_cell_volume        2390.0(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7021822