The first hafnium methandiide complexes: the assembly of an entire triad of group 4 metal ‘pincer’ bis(phosphinimine) complexes possessing the MC carbene‒ylide structure
Kamalesh Babu, Ruppa P.; Cavell, Ronald G.; McDonald, Robert; Chemical Communications  (2000) 481–; doi:10.1039/a909771f

data_7110818
_publ_section_title
;
 The first hafnium methandiide complexes: the assembly of an entire triad
 of group 4 metal &#x2018;pincer&#x2019; bis(phosphinimine) complexes
 possessing the M&#xE006;C carbene--ylide structure
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              481
_journal_paper_doi               10.1039/a909771f
_journal_year                    2000
_chemical_formula_sum            'C31 H62 Cl2 Hf N2 P2 Si2'
_chemical_formula_weight         830.34
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.226(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3572(7)
_cell_length_b                   20.8156(10)
_cell_length_c                   17.8865(10)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      27.50
_cell_volume                     3850.1(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5204
_diffrn_reflns_theta_max         57.39
_diffrn_reflns_theta_min         3.26
_diffrn_standards_interval_count 297
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.829
_exptl_absorpt_correction_T_max  .1169
_exptl_absorpt_correction_T_min  .0275
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.652
_refine_diff_density_min         -.928
_refine_diff_density_rms         .102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4863
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0735P)^2^+3.4829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1148
_refine_ls_wR_factor_obs         0.1100
_reflns_number_observed          4306
_reflns_number_total             4864
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a909771fsup1.cif
_cod_data_source_block           rgc9810
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0735P)^2^+3.4829P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0735P)^2^+3.4829P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110818