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_7033695
_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         'C7 H8 B1 N1 O4'
_chemical_formula_sum            'C7 H8 B N O4'
_chemical_formula_weight         180.96
_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             13-07-29
_audit_creation_method           CRYSTALS_ver_14.23
_audit_update_record
;
2014-12-03 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.726(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2422(5)
_cell_length_b                   11.9040(11)
_cell_length_c                   11.5004(9)
_cell_measurement_reflns_used    4078
_cell_measurement_temperature    200
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2.26
_cell_volume                     854.49(12)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7616
_diffrn_reflns_theta_full        25.088
_diffrn_reflns_theta_max         25.088
_diffrn_reflns_theta_min         3.423
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/pentane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9350
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1504
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.0029076
_refine_ls_shift/su_mean         0.0006122
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 1.13P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1944
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1944
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                807
_reflns_number_total             1509
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.22
_oxford_diffrn_Wilson_scale      7.08
_oxford_refine_ls_r_factor_ref   0.1427
_oxford_refine_ls_scale          0.548(6)
_oxford_reflns_number_all        1504
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CS002b At 11:36 on 27/ 7'
_cod_data_source_file            c4dt03695f1.cif
_cod_data_source_block           CS002b
_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        'C7 H8 B1 N1 O4'
_cod_database_code               7033695
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.01 = C(3) TO C(5) 
U(IJ) 0.0, 0.01 = C(4) TO C(6) 
U(IJ) 0.0, 0.01 = N(1) TO C(5) 
U(IJ) 0.0, 0.005 = N(1) TO C(6) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;