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_4087835
_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         'C62 H54 Br1 O2.50 P3 Si1 W1'
_chemical_formula_sum            'C62 H54 Br O2.5 P3 Si W'
_chemical_formula_weight         1223.87
_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             14-03-27
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 94.3896(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2616(2)
_cell_length_b                   18.3376(2)
_cell_length_c                   19.1608(2)
_cell_measurement_reflns_used    184906
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.55
_cell_volume                     5346.63(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            117855
_diffrn_reflns_theta_full        30.034
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         2.594
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.065
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.040
_refine_diff_density_max         5.09
_refine_diff_density_min         -2.78
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9326
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         15628
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.0043892
_refine_ls_shift/su_mean         0.0000298
_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: 
 20.3 28.8 14.0 3.58 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1313
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1313
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                11743
_reflns_number_total             15632
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.39
_oxford_diffrn_Wilson_scale      64.83
_oxford_refine_ls_r_factor_ref   0.0747
_oxford_refine_ls_scale          0.14662(4)
_oxford_reflns_number_all        15628
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'JX038 At 11:42 on 27/ 3'
_cod_data_source_file            om5b00635_si_002.cif
_cod_data_source_block           Comp_3c
_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 21/c '
_cod_original_formula_sum        'C62 H54 Br1 O2.50 P3 Si1 W1'
_cod_database_code               4087835
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
REM CONT O(31, OCC) 
REM CONT BR(1, U'S) UNTIL C(96) 
REM CONT C(221, U[ISO]) UNTIL C(262) 
REM CONT C(221, OCC) C(222, OCC) 
REM CONT C(231, OCC) C(232, OCC) 
REM CONT C(241, OCC) C(242, OCC) 
REM CONT C(251, OCC) C(252, OCC) 
REM CONT C(261, OCC) C(262, OCC) 
REM EQUIV C(221, OCC) C(222, OCC) 
REM CONT C(231, OCC) C(232, OCC) 
REM CONT C(241, OCC) C(242, OCC) 
REM CONT C(251, OCC) C(252, OCC) 
REM CONT C(261, OCC) C(262, OCC) 
REM WEIGHT -1 C(222, OCC) C(232, OCC) 
REM CONT C(242, OCC) C(252, OCC) C(262, OCC) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM U(IJ) 0.0, 0.01 = C(21) TO C(22) 
REM U(IJ) 0.0, 0.01 = C(22) TO C(23) 
REM U(IJ) 0.0, 0.01 = C(23) TO C(24) 
REM U(IJ) 0.0, 0.01 = C(24) TO C(25) 
REM U(IJ) 0.0, 0.01 = C(25) TO C(26) 
REM U(IJ) 0.0, 0.01 = C(26) TO C(21) 
REM 
LIMIT C(242,U[12]) 
LIMIT C(232,U[23]) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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