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_7033701
_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         'C49 H49 B1 N2 O5 P2 Ru1 S2, C3 H6 O1'
_chemical_formula_sum            'C52 H55 B N2 O6 P2 Ru S2'
_chemical_formula_weight         1041.98
_space_group_IT_number           14
_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     other
_audit_creation_date             2014-08-02
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2014-12-03 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.700(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   12.8444(4)
_cell_length_b                   25.1664(7)
_cell_length_c                   47.1159(13)
_cell_measurement_reflns_used    3398
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     15223.4(8)
_computing_cell_refinement       'CrysAlis PRO, (Agilent Technologies, 2013)'
_computing_data_collection       'SuperNova, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis PRO, (Agilent Technologies, 2013)'
_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 0.965
_diffrn_measured_fraction_theta_max 0.899
_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     1.54180
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            43623
_diffrn_reflns_theta_full        25.298
_diffrn_reflns_theta_max         72.281
_diffrn_reflns_theta_min         3.541
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.266
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6480
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone/pentane'
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.82
_refine_diff_density_min         -1.52
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9723
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1797
_refine_ls_number_reflns         26923
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.0027757
_refine_ls_shift/su_mean         0.0000551
_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: 
 0.126E+04 0.144E+04 869. 327. 49.9 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1682
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1680
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              57
_reflns_limit_l_min              0
_reflns_number_gt                16072
_reflns_number_total             27038
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.79
_oxford_diffrn_Wilson_scale      1.84
_oxford_refine_ls_r_factor_ref   0.1437
_oxford_refine_ls_scale          0.8183(13)
_oxford_reflns_number_all        26926
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'C:\Users\Hill Group\Desktop\Jas At 13:39 on '
_cod_data_source_file            c4dt03695f1.cif
_cod_data_source_block           jas158(JSW383)
_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 21/n '
_cod_original_formula_sum        'C52 H55 B1 N2 O6 P2 Ru1 S2'
_cod_database_code               7033701
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
REM CONT B(1, U'S) UNTIL C(213) 
REM CONT C(214, U[ISO]) UNTIL C(217) 
REM CONT C(221, U'S) UNTIL C(503) 
REM CONT C(214, OCC) C(215, OCC) C(216, OCC) C(217, OCC) 
REM EQUIV C(214, OCC) C(215, OCC) C(216, OCC) C(217, OCC) 
REM WEIGHT -1 C(214, OCC) C(215, OCC) 
REM 
FIX C(216, U[23]) 
FIX C(216, U[13]) 
FIX C(216, Y) 
FIX C(216, U[11]) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM 
REM U(IJ) 0.0 0.005 C(214) TO C(216) 
REM U(IJ) 0.0 0.01 C(215) TO C(217) 
REM 
REM LIMIT C(216, U[23]) 
REM LIMIT C(216, U[13]) 
REM LIMIT C(216, Y) 
REM LIMIT C(216, U[11]) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;