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_7701158
_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         'C80 H60 Cl2 O4 P4 Ru2, 2(C1 H2 Cl2)'
_chemical_formula_sum            'C82 H64 Cl6 O4 P4 Ru2'
_chemical_formula_weight         1652.16
_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     other
_audit_creation_date             14-11-16
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2014-11-17 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.705(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.361(5)
_cell_length_b                   10.355(5)
_cell_length_c                   29.764(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     7779(4)
_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      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       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            112255
_diffrn_reflns_theta_full        24.110
_diffrn_reflns_theta_max         24.110
_diffrn_reflns_theta_min         1.613
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.101
_platon_squeeze_details
;
;
_refine_diff_density_max         5.57
_refine_diff_density_min         -1.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9676
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         12357
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.0016661
_refine_ls_shift/su_mean         0.0000491
_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: 
 43.2 67.2 33.0 8.04 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2300
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2300
_reflns_limit_h_max              29
_reflns_limit_h_min              -31
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                9079
_reflns_number_total             12367
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.67
_oxford_diffrn_Wilson_scale      92.13
_oxford_refine_ls_r_factor_ref   0.1026
_oxford_refine_ls_scale          0.10251(5)
_oxford_reflns_number_all        12357
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'sir: ---- maxus'
_cod_data_source_file            c9dt03229k2.cif
_cod_data_source_block           mb11(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 21/c '
_cod_database_code               7701158
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM 
U(IJ) 0.0, 0.02 = C(201) TO CL(201) 
U(IJ) 0.0, 0.02 = C(201) TO CL(202) 
REM 
U(IJ) 0.0, 0.01 = C(301) TO CL(301) 
U(IJ) 0.0, 0.01 = C(301) TO CL(302) 
REM 
REM U(IJ) 0.0, 0.01 = C(401) TO CL(401) 
REM U(IJ) 0.0, 0.01 = C(401) TO CL(402) 
REM U(IJ) 0.0, 0.01 = CL(401) TO CL(402) 
REM 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;