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_7701157
_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         '2(C47 H49 Cl1 O1 P2 Ru1 Si2)'
_chemical_formula_sum            'C94 H98 Cl2 O2 P4 Ru2 Si4'
_chemical_formula_weight         1769.09
_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_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-07-30
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2015-07-30 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.300(3)
_cell_length_b                   35.950(7)
_cell_length_c                   20.730(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     8943(3)
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            146381
_diffrn_reflns_theta_full        25.131
_diffrn_reflns_theta_max         25.131
_diffrn_reflns_theta_min         1.155
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_refine_diff_density_max         2.08
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9246
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         15596
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.0012508
_refine_ls_shift/su_mean         0.0000428
_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: 
 10.7 15.9 7.52 1.88 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1201
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1201
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              42
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                12026
_reflns_number_total             15670
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0636
_oxford_refine_ls_scale          0.098688(19)
_oxford_reflns_number_all        15596
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mb2 in P2(1)/c'
_cod_data_source_file            c9dt03229k2.cif
_cod_data_source_block           mb2(JasRedo)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               7701157
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
FIX C(17, U[33]) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.02 = SI(1) TO C(12) 
REM U(IJ) 0.0, 0.02 = SI(2) TO C(17) 
REM U(IJ) 0.0, 0.02 = C(16) TO C(17) 
REM 
REM LIMIT C(17, U[33]) 
REM 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;