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_7033705
_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(C1 H1 Cl3)'
_chemical_formula_sum            'C44 H42 Cl7 N O P2 Ru S2'
_chemical_formula_weight         1076.14
_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             14-06-27
_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                66.3796(16)
_cell_angle_beta                 77.3401(15)
_cell_angle_gamma                88.4075(14)
_cell_formula_units_Z            2
_cell_length_a                   9.90371(17)
_cell_length_b                   15.5276(3)
_cell_length_c                   18.2972(3)
_cell_measurement_reflns_used    20953
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      5
_cell_volume                     2509.67(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30901
_diffrn_reflns_theta_full        72.295
_diffrn_reflns_theta_max         72.295
_diffrn_reflns_theta_min         3.113
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.598
_exptl_absorpt_correction_T_max  0.35
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform/hexane'
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.140
_platon_squeeze_details
;
;
_refine_diff_density_max         1.12
_refine_diff_density_min         -1.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9016
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9838
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.0003791
_refine_ls_shift/su_mean         0.0000145
_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: 
 0.230E+04 0.377E+04 0.242E+04 0.107E+04 295. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0818
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0818
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              -17
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                9682
_reflns_number_total             9887
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.72
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_r_factor_ref   0.0356
_oxford_refine_ls_scale          4.09(3)
_oxford_reflns_number_all        9838
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title
'THIS IS THE DEFAULT SETTING FOR THE TITLE, P'
_cod_data_source_file            c4dt03695f1.cif
_cod_data_source_block           jas149
_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        'C44 H42 Cl7 N1 O1 P2 Ru1 S2'
_cod_database_code               7033705
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
REM CONT CL(1, U[ISO]) UNTIL CL(2) 
REM CONT CL(101, U'S) UNTIL N(1) 
REM CONT O(1, U[ISO]) UNTIL O(2) 
REM CONT P(1, U'S) UNTIL S(2) 
REM CONT C(1, U[ISO]) UNTIL C(2) 
REM CONT C(3, U'S) UNTIL C(201) 
REM CONT CL(1, OCC) O(1, OCC) C(1, OCC) 
REM CONT CL(2, OCC) O(2, OCC) C(2, OCC) 
REM EQUIV CL(1, OCC) O(1, OCC) C(1, OCC) 
REM CONT CL(2, OCC) O(2, OCC) C(2, OCC) 
REM WEIGHT -1 CL(2, OCC) O(2, OCC) C(2, OCC) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;