Organometallic chemistry of ethynyl boronic acid MIDA ester, HC[triple bond, length as m-dash]CB(O2CCH2)2NMe.
Hill, Anthony F.; Stewart, Craig D.; Ward, Jas S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 5713–5726; doi:10.1039/c4dt03695f

data_7033703
_publ_section_title
;
 Organometallic chemistry of ethynyl boronic acid MIDA ester, HC[triple
 bond, length as m-dash]CB(O2CCH2)2NMe.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5713
_journal_page_last               5726
_journal_paper_doi               10.1039/c4dt03695f
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C42 H40 Cl1 N1 O1 P2 Ru1 S2, 2.5(C6 H6)'
_chemical_formula_sum            'C57 H55 Cl N O P2 Ru S2'
_chemical_formula_weight         1032.67
_space_group_IT_number           2
_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             14-07-17
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2014-12-03 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                83.116(6)
_cell_angle_beta                 76.954(5)
_cell_angle_gamma                85.934(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9889(5)
_cell_length_b                   14.4392(12)
_cell_length_c                   17.9821(13)
_cell_measurement_reflns_used    3452
_cell_measurement_temperature    150
_cell_measurement_theta_max      69
_cell_measurement_theta_min      3
_cell_volume                     2505.9(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      150
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13864
_diffrn_reflns_theta_full        33.660
_diffrn_reflns_theta_max         70.125
_diffrn_reflns_theta_min         3.086
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.715
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1070
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/hexane'
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.021
_refine_diff_density_max         4.77
_refine_diff_density_min         -2.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0523
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8915
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.1175
_refine_ls_shift/su_max          0.0006582
_refine_ls_shift/su_mean         0.0000307
_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: 
 0.643E+04 0.766E+04 0.471E+04 0.207E+04 118. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2778
_refine_ls_wR_factor_gt          0.2679
_refine_ls_wR_factor_ref         0.2778
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                6797
_reflns_number_total             8969
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.1413
_oxford_refine_ls_scale          4.55(12)
_oxford_reflns_number_all        8915
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title
'C:\Users\Jas\Desktop\jas152(JSW3 At 21:47 on'
_cod_data_source_file            c4dt03695f1.cif
_cod_data_source_block           jas152(JSW367)(5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 7033695--7033706.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C57 H55 Cl1 N1 O1 P2 Ru1 S2'
_cod_database_code               7033703
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
REM CONT CL(1, U'S) UNTIL S(2) 
REM CONT C(1, U[ISO]) 
REM CONT C(2, U'S) UNTIL C(303) 
REM CONT C(1, OCC) O(1, OCC) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM 
U(IJ) 0.0, 0.01 = C(51) TO C(52) 
U(IJ) 0.0, 0.01 = C(51) TO C(53) 
REM 
PLANAR C(201) UNTIL C(206) 
REM 
DIST 0.0, 0.005 = MEAN C(201) TO C(202), C(202) TO C(203) 
DIST 0.0, 0.005 = MEAN C(202) TO C(203), C(203) TO C(204) 
DIST 0.0, 0.005 = MEAN C(203) TO C(204), C(204) TO C(205) 
DIST 0.0, 0.005 = MEAN C(204) TO C(205), C(205) TO C(206) 
DIST 0.0, 0.005 = MEAN C(205) TO C(206), C(206) TO C(201) 
DIST 0.0, 0.005 = MEAN C(206) TO C(201), C(201) TO C(202) 
REM 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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