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_7701160
_publ_section_title
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 Hydrogenating an Organometallic Carbon Chain: Buten-yn-diyl (CH=CHC\\tb
 C) as a Missing Link
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03229K
_journal_year                    2019
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C43 H39 Cl1 O2 P2 Ru1 Si1'
_chemical_formula_sum            'C43 H39 Cl O2 P2 Ru Si'
_chemical_formula_weight         814.34
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.55(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.970(2)
_cell_length_b                   19.640(4)
_cell_length_c                   19.770(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     3859.0(14)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.038
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            76722
_diffrn_reflns_theta_full        27.496
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.584
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9335
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8817
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.0008874
_refine_ls_shift/su_mean         0.0000400
_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: 
 40.2 63.8 37.2 15.2 3.45 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0925
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0925
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7972
_reflns_number_total             8839
_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   0.0417
_oxford_refine_ls_scale          0.3673(3)
_oxford_reflns_number_all        8817
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mb3 in P2(1)/n'
_cod_data_source_file            c9dt03229k2.cif
_cod_data_source_block           mb3(JasRedo)
_cod_original_cell_volume        3859.0(13)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C43 H39 Cl1 O2 P2 Ru1 Si1'
_cod_database_code               7701160
_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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REM 
U(IJ) 0.0, 0.01 = C(5) TO C(6) 
U(IJ) 0.0, 0.01 = C(6) TO C(7) 
U(IJ) 0.0, 0.01 = C(7) TO C(5) 
REM 
U(IJ) 0.0, 0.03 = C(211) TO C(212) 
U(IJ) 0.0, 0.03 = C(212) TO C(213) 
U(IJ) 0.0, 0.03 = C(213) TO C(214) 
U(IJ) 0.0, 0.03 = C(214) TO C(215) 
U(IJ) 0.0, 0.03 = C(215) TO C(216) 
U(IJ) 0.0, 0.03 = C(216) TO C(211) 
REM 
END                                                                             
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