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_4087837
_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         'C29 H49 Br1 O2 P2 W1, 0.5(C6 H14)'
_chemical_formula_sum            'C32 H56 Br O2 P2 W'
_chemical_formula_weight         798.50
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-05-26
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 94.9140(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.90890(10)
_cell_length_b                   14.50190(10)
_cell_length_c                   19.51290(10)
_cell_measurement_reflns_used    45934
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     3357.52(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66122
_diffrn_reflns_theta_full        72.312
_diffrn_reflns_theta_max         72.312
_diffrn_reflns_theta_min         3.725
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.861
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.56
_refine_diff_density_min         -1.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9524
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6606
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.0019604
_refine_ls_shift/su_mean         0.0001098
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.184E+04 0.281E+04 0.175E+04 718. 125. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0574
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0574
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                6543
_reflns_number_total             6633
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.78
_oxford_diffrn_Wilson_scale      0.15
_oxford_refine_ls_r_factor_ref   0.0272
_oxford_refine_ls_scale          2.814(11)
_oxford_reflns_number_all        6606
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title
'C:\Users\Jas\Desktop\JX048\JX048 At 19:22 on'
_cod_data_source_file            om5b00635_si_002.cif
_cod_data_source_block           Comp_4
_cod_depositor_comments
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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 21/c '
_cod_original_formula_sum        'C32 H56 Br1 O2 P2 W1'
_cod_database_code               4087837
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0  , .02 =      C(101) TO C(102) 
U(IJ) 0.0  , .02 =      C(102) TO C(103) 
U(IJ) 0.0  , .02 =      C(103) TO C(101) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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