Synthesis of a Stable Methylidyne Complex
Hill, Anthony F.; Ward, Jas S.; Xiong, Yaoyao; Organometallics 34 (2015) 5057–; doi:10.1021/acs.organomet.5b00635

data_4087833
_publ_section_title
;
 Synthesis of a Stable Methylidyne Complex
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5057
_journal_paper_doi               10.1021/acs.organomet.5b00635
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C33 H29 Br1 N2 O2 Si1 W1'
_chemical_formula_sum            'C33 H29 Br N2 O2 Si W'
_chemical_formula_weight         777.44
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-05-02
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                63.067(3)
_cell_angle_beta                 76.1846(19)
_cell_angle_gamma                79.043(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8049(3)
_cell_length_b                   11.8059(4)
_cell_length_c                   12.5211(3)
_cell_measurement_reflns_used    11203
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      4
_cell_volume                     1503.98(8)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'Ortep-3 for windows (Farrugia, 1997)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15701
_diffrn_reflns_theta_full        70.966
_diffrn_reflns_theta_max         72.415
_diffrn_reflns_theta_min         3.873
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.310
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.50
_refine_diff_density_min         -2.12
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0247
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5914
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.0011263
_refine_ls_shift/su_mean         0.0000254
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 1.62P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0599
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0599
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -12
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                5716
_reflns_number_total             5939
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.64
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0238
_oxford_refine_ls_scale          3.85(3)
_oxford_reflns_number_all        5914
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title
'C:\Users\Jas\Desktop\JX039\JX039 At 20:40 on'
_cod_data_source_file            om5b00635_si_002.cif
_cod_data_source_block           Comp_2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C33 H29 Br1 N2 O2 Si1 W1'
_cod_database_code               4087833
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;