Hydrogenating an Organometallic Carbon Chain: Buten-yn-diyl (CH=CHC\τb C) as a Missing Link
Hill, Anthony; Bartlett, Michael J.; Sharma, Manab; Smith, Matthew K.; Ward, Jas S.; Dalton Transactions  (2019) –; doi:10.1039/C9DT03229K

data_7701156
_publ_section_title
;
 Hydrogenating an Organometallic Carbon Chain: Buten-yn-diyl (CH=CHC\\tb
 C) as a Missing Link
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03229K
_journal_year                    2019
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C50 H55 N1 O1 P2 Ru1 S2 Si2'
_chemical_formula_sum            'C50 H55 N O P2 Ru S2 Si2'
_chemical_formula_weight         969.31
_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_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             15-07-31
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2015-07-31 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                80.940(5)
_cell_angle_beta                 71.440(5)
_cell_angle_gamma                83.977(5)
_cell_formula_units_Z            2
_cell_length_a                   12.434(5)
_cell_length_b                   13.181(5)
_cell_length_c                   17.570(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    173
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     2691.1(17)
_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    '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      173
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.078
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23261
_diffrn_reflns_theta_full        26.101
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         2.912
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.260
_platon_squeeze_details
;
;
_refine_diff_density_max         2.84
_refine_diff_density_min         -1.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9931
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         12202
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.0009162
_refine_ls_shift/su_mean         0.0000278
_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: 
 48.0 73.0 37.0 9.95 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1925
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.1924
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                10547
_reflns_number_total             12238
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.83
_oxford_diffrn_Wilson_scale      8.35
_oxford_refine_ls_r_factor_ref   0.0734
_oxford_refine_ls_scale          0.5478(11)
_oxford_reflns_number_all        12209
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'sir: ---- maxus'
_cod_data_source_file            c9dt03229k2.cif
_cod_data_source_block           mb4(JasRedo)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C50 H55 N1 O1 P2 Ru1 S2 Si2'
_cod_database_code               7701156
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
REM 
REM FIX SI(2, U[22]) 
FIX SI(2, U[11]) 
FIX SI(2, U[33]) 
REM 
FIX C(18, U[22]) 
FIX C(18, U[11]) 
FIX C(18, U[33]) 
REM 
FIX C(19, U[22]) 
FIX C(19, U[11]) 
FIX C(19, U[33]) 
REM 
FIX C(20, U[22]) 
FIX C(20, U[11]) 
FIX C(20, U[33]) 
REM 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM 
LIMIT SI(2, U[22]) 
REM LIMIT SI(2, U[11]) 
REM LIMIT SI(2, U[33]) 
REM 
REM LIMIT C(18, U[22]) 
REM LIMIT C(18, U[11]) 
REM LIMIT C(18, U[33]) 
REM 
REM LIMIT C(19, U[22]) 
REM LIMIT C(19, U[11]) 
REM LIMIT C(19, U[33]) 
REM 
REM LIMIT C(20, U[22]) 
REM LIMIT C(20, U[11]) 
REM LIMIT C(20, U[33]) 
REM 
ANGLE 0.0, 1. = MEAN C(18) TO SI(2) TO C(19), C(19) TO SI(2) TO C(20) 
ANGLE 0.0, 1. = MEAN C(19) TO SI(2) TO C(20), C(20) TO SI(2) TO C(18) 
ANGLE 0.0, 1. = MEAN C(20) TO SI(2) TO C(18), C(18) TO SI(2) TO C(19) 
REM 
U(IJ) 0.0, 0.01 = C(111) TO C(112) 
U(IJ) 0.0, 0.01 = C(112) TO C(113) 
U(IJ) 0.0, 0.01 = C(113) TO C(114) 
U(IJ) 0.0, 0.01 = C(114) TO C(115) 
U(IJ) 0.0, 0.01 = C(115) TO C(116) 
U(IJ) 0.0, 0.01 = C(116) TO C(111) 
REM 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;