Synthesis, characterisation, and dehydrocoupling ability of zirconium complexes bearing hindered bis(amido)silyl ligands.
Lummis, Paul A.; McDonald, Robert; Ferguson, Michael J.; Rivard, Eric; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7009–7020; doi:10.1039/c5dt00306g

data_7034306
_publ_section_title
;
 Synthesis, characterisation, and dehydrocoupling ability of zirconium
 complexes bearing hindered bis(amido)silyl ligands.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7009
_journal_page_last               7020
_journal_paper_doi               10.1039/c5dt00306g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C37 H66 B2 N4 Si Zr,0.5(C4 H8 O)'
_chemical_formula_sum            'C39 H70 B2 N4 O0.5 Si Zr'
_chemical_formula_weight         743.92
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8302(4)
_cell_length_b                   16.9778(7)
_cell_length_c                   23.5656(9)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.22
_cell_measurement_theta_min      2.23
_cell_volume                     4330.4(3)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34513
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_correction_T_min  0.8671
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered or 
partial-occupancy solvent tetrahydrofuran oxygen or carbon atoms were 
unsuccessful.  The data were corrected for disordered electron density 
through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. 
Acta Crystallogr. 1990, A46, 194201) as implemented in PLATON (Spek, 
A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 
36, 713.  PLATON - a multipurpose crystallographic tool.  Utrecht 
University, Utrecht, The Netherlands).  A total solvent-accessible void 
volume of 525 3 with a total electron count of 83 (consistent with 2 
molecules of solvent tetrahydrofuran, or 0.5 molecules per formula unit 
of the [{iPr2Si(NSiPh3)2}Zr(BH4)2(4-Me2N-pyridine)] molecule) was found 
in the unit cell
;
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8913
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.6651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                7012
_reflns_number_total             8913
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5dt00306g2.cif
_cod_data_source_block           riv1267
_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/RSC/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 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 7034303--7034308.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C39 H70 B2 N4 O0.50 Si Zr'
_cod_database_code               7034306