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_7701155
_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         'C40 H31 Cl1 O2 P2 Ru1'
_chemical_formula_sum            'C40 H31 Cl O2 P2 Ru'
_chemical_formula_weight         742.15
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-09-24
_audit_creation_method           CRYSTALS_ver_14.23
_audit_update_record
;
2014-11-15 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.900(5)
_cell_length_b                   10.450(2)
_cell_length_c                   29.670(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.55
_cell_volume                     7251(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    '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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.084
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            58229
_diffrn_reflns_theta_full        25.130
_diffrn_reflns_theta_max         25.130
_diffrn_reflns_theta_min         2.982
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
;
_refine_diff_density_max         1.28
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0134
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6467
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.0016370
_refine_ls_shift/su_mean         0.0000445
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +20.32P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1480
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1480
_reflns_limit_h_max              27
_reflns_limit_h_min              -28
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                5415
_reflns_number_total             6467
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.61
_oxford_diffrn_Wilson_scale      55.35
_oxford_refine_ls_r_factor_ref   0.0629
_oxford_refine_ls_scale          0.14622(9)
_oxford_reflns_number_all        6467
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mb12 in C2/c'
_cod_data_source_file            c9dt03229k2.cif
_cod_data_source_block           mb12(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      'C 2/c '
_cod_original_formula_sum        'C40 H31 Cl1 O2 P2 Ru1'
_cod_database_code               7701155
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
REM CONT CL(1, U'S) UNTIL C(2) 
REM CONT C(3, U[ISO]) C(4, U[ISO]) C(5, U[ISO]) C(6, U[ISO]) 
REM CONT C(11, U'S) UNTIL C(66) 
REM 
REM CONT CL(1, U'S) UNTIL O(2) 
REM CONT O(101, U[ISO]) 
REM CONT P(1, U'S) UNTIL C(66) 
REM CONT C(101, U[ISO]) UNTIL C(102) 
REM CONT O(101, OCC) C(101, OCC) C(102, OCC) 
REM 
FIX C(3, U[33]) 
FIX C(5, U[33]) 
FIX C(3, U[22]) 
FIX C(4, U[23]) 
REM FIX C(5,U[33]) 
REM FIX C(4,U[23]) 
REM FIX C(4, Z) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.02 = C(3) TO C(5) 
U(IJ) 0.0, 0.01 = C(4) TO C(6) 
REM 
REM ANGLE 170.0, 5. = C(3) TO C(4) TO C(6,-2,1,1,0,1) 
REM 
REM LIMIT C(5, U[33]) 
REM LIMIT C(3, U[33]) 
REM LIMIT C(3, U[22]) 
REM LIMIT C(4, U[23]) 
LIMIT C(3, Z) 
LIMIT C(4, X) 
LIMIT C(5, Y) 
REM 
PLANAR C(51) UNTIL C(56) 
DIST 0.0, 0.01 = MEAN C(51) TO C(52), C(52) TO C(53) 
DIST 0.0, 0.01 = MEAN C(52) TO C(53), C(53) TO C(54) 
DIST 0.0, 0.01 = MEAN C(53) TO C(54), C(54) TO C(55) 
DIST 0.0, 0.01 = MEAN C(54) TO C(55), C(55) TO C(56) 
DIST 0.0, 0.01 = MEAN C(55) TO C(56), C(56) TO C(51) 
DIST 0.0, 0.01 = MEAN C(56) TO C(51), C(51) TO C(52) 
REM 
U(IJ) 0.0, 0.02 = C(61) TO C(62) 
U(IJ) 0.0, 0.02 = C(62) TO C(63) 
U(IJ) 0.0, 0.02 = C(63) TO C(64) 
U(IJ) 0.0, 0.02 = C(64) TO C(65) 
U(IJ) 0.0, 0.02 = C(65) TO C(66) 
U(IJ) 0.0, 0.02 = C(66) TO C(61) 
REM 
REM PLANAR C(61) UNTIL C(66) 
DIST 0.0, 0.005 = MEAN C(61) TO C(62), C(62) TO C(63) 
DIST 0.0, 0.005 = MEAN C(62) TO C(63), C(63) TO C(64) 
DIST 0.0, 0.005 = MEAN C(63) TO C(64), C(64) TO C(65) 
DIST 0.0, 0.005 = MEAN C(64) TO C(65), C(65) TO C(66) 
DIST 0.0, 0.005 = MEAN C(65) TO C(66), C(66) TO C(61) 
DIST 0.0, 0.005 = MEAN C(66) TO C(61), C(61) TO C(62) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;