Binary role of an ylide in formation of a terminal methylidene complex of niobium
Keith Searles; Karlijn Keijzer; Chun-Hsing Chen; Mu-Hyun Baik; Daniel J. Mindiola; Chem.Commun. 50 (2014) 6267–; doi:10.1039/C4CC01404A

data_7113944
_publ_section_title
;
 Binary role of an ylide in formation of a terminal methylidene complex of
 niobium
;
_journal_name_full               Chem.Commun.
_journal_page_first              6267
_journal_paper_doi               10.1039/C4CC01404A
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C110.00 H104.50 Nb1 O3 P1'
_chemical_formula_sum            'C110 H104.5 Nb O3 P'
_chemical_formula_weight         1598.43
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-05-15
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 102.424(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8662(16)
_cell_length_b                   39.237(4)
_cell_length_c                   15.5681(16)
_cell_measurement_reflns_used    9235
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     8868.3(16)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58726
_diffrn_reflns_theta_full        25.162
_diffrn_reflns_theta_max         25.162
_diffrn_reflns_theta_min         1.038
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3378.000
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9776
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1984
_refine_ls_number_reflns         27007
_refine_ls_number_restraints     363
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.0236343
_refine_ls_shift/su_mean         0.0014162
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +10.90P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1235
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1235
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              43
_reflns_limit_k_min              -46
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                23424
_reflns_number_total             27140
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.02
_oxford_diffrn_Wilson_scale      272.27
_oxford_refine_ls_r_factor_ref   0.0551
_oxford_refine_ls_scale          0.064058(7)
_oxford_reflns_number_all        27007
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title '13032 in P2(1)'
_cod_data_source_file            c4cc01404a2.cif
_cod_data_source_block           13032
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C110.00 H104.50 Nb1 O3 P1'
_cod_database_code               7113944