Synthesis and Characterization of Crystalline Structures Based on Phenylboronate Ligands Bound to Alkaline Earth Cations
Marc Reinholdt; Jonas Croissant; Lidia Di Carlo; Dominique Granier; Philippe Gaveau; Sylvie Bégu; Jean-Marie Devoisselle; P. Hubert Mutin; Mark E. Smith; Christian Bonhomme; Christel Gervais; Arie van der Lee; Danielle Laurencin; Inorganic Chemistry 50 (2011) 7802–7810; doi:10.1021/ic200961a

data_4325937
_publ_contact_author_address
;
 Chemical Crystallography Laboratory,
 Department of Chemistry,
 University of Nowhere,
 Nowhere, NO1 4T, UK.
;
_publ_contact_author_email       dlaurenc@univ-montp2.fr
_publ_contact_author_name        'Danielle Laurencin'
_publ_section_title
;
 Synthesis and Characterization of Crystalline Structures Based on
 Phenylboronate Ligands Bound to Alkaline Earth Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7802
_journal_page_last               7810
_journal_paper_doi               10.1021/ic200961a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C12 H18 B2 O7 Sr1'
_chemical_formula_sum            'C12 H18 B2 O7 Sr'
_chemical_formula_weight         383.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-12-02
_audit_creation_method           CRYSTALS_ver_14.11
_audit_update_record
;
2011-02-23 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 92.783(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.21861(17)
_cell_length_b                   7.9567(2)
_cell_length_c                   30.7635(11)
_cell_measurement_reflns_used    7344
_cell_measurement_temperature    175
_cell_measurement_theta_max      29.0290
_cell_measurement_theta_min      2.8772
_cell_volume                     1520.37(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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      175
_diffrn_detector_area_resol_mean 8.4205
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            17800
_diffrn_reflns_theta_full        26.766
_diffrn_reflns_theta_max         29.093
_diffrn_reflns_theta_min         2.883
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.70
_refine_diff_density_min         -4.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.0001396
_refine_ls_shift/su_mean         0.0000103
_refine_ls_structure_factor_coef F
_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: 
 6.54 -7.34 3.05 -0.586 -0.993 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0657
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0640
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                3232
_reflns_number_total             3711
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0927
_oxford_refine_ls_scale          0.9187(19)
_oxford_reflns_number_all        3711
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ic200961a_si_003.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '    -P 2ybc'
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C12 H18 B2 O7 Sr1'
_cod_database_code               4325937
_cell_oxdiff_length_a            6.21731(16)
_cell_oxdiff_length_b            7.95687(19)
_cell_oxdiff_length_c            30.7692(10)
_cell_oxdiff_angle_alpha         89.986(2)
_cell_oxdiff_angle_beta          92.776(2)
_cell_oxdiff_angle_gamma         89.997(2)
_cell_oxdiff_volume              1520.37(7)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 91.0
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE O   (   4,X'S) H   (  41,X'S) 
RIDE O   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE O   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE O   (  13,X'S) H   ( 131,X'S)
RIDE O   (  15,X'S) H   ( 151,X'S) 
RIDE O   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(2) TO B(3) 
VIBR .0, 0.00200 = B(3) TO O(4) 
VIBR .0, 0.00200 = B(3) TO O(5) 
VIBR .0, 0.00200 = B(3) TO C(6) 
VIBR .0, 0.00500 = O(4) TO O(2) 
VIBR .0, 0.00500 = O(5) TO O(2) 
VIBR .0, 0.00500 = O(5) TO O(4) 
VIBR .0, 0.00500 = C(6) TO O(2) 
VIBR .0, 0.00500 = C(6) TO O(4) 
VIBR .0, 0.00500 = C(6) TO O(5) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00200 = C(6) TO C(11) 
VIBR .0, 0.00500 = C(7) TO B(3) 
VIBR .0, 0.00500 = C(11) TO B(3) 
VIBR .0, 0.00500 = C(11) TO C(7) 
VIBR .0, 0.00200 = C(7) TO C(8) 
VIBR .0, 0.00500 = C(8) TO C(6) 
VIBR .0, 0.00200 = C(8) TO C(9) 
VIBR .0, 0.00500 = C(9) TO C(7) 
VIBR .0, 0.00200 = C(9) TO C(10) 
VIBR .0, 0.00500 = C(10) TO C(8) 
VIBR .0, 0.00200 = C(10) TO C(11) 
VIBR .0, 0.00500 = C(11) TO C(9) 
VIBR .0, 0.00500 = C(10) TO C(6) 
VIBR .0, 0.00200 = O(13) TO B(14) 
VIBR .0, 0.00200 = B(14) TO O(15) 
VIBR .0, 0.00200 = B(14) TO O(16)
VIBR .0, 0.00200 = B(14) TO C(17) 
VIBR .0, 0.00500 = O(15) TO O(13) 
VIBR .0, 0.00500 = O(16) TO O(13) 
VIBR .0, 0.00500 = O(16) TO O(15) 
VIBR .0, 0.00500 = C(17) TO O(13) 
VIBR .0, 0.00500 = C(17) TO O(15) 
VIBR .0, 0.00500 = C(17) TO O(16) 
VIBR .0, 0.00200 = C(17) TO C(18) 
VIBR .0, 0.00200 = C(17) TO C(22) 
VIBR .0, 0.00500 = C(18) TO B(14) 
VIBR .0, 0.00500 = C(22) TO B(14) 
VIBR .0, 0.00500 = C(22) TO C(18) 
VIBR .0, 0.00200 = C(18) TO C(19) 
VIBR .0, 0.00500 = C(19) TO C(17) 
VIBR .0, 0.00200 = C(19) TO C(20) 
VIBR .0, 0.00500 = C(20) TO C(18) 
VIBR .0, 0.00200 = C(20) TO C(21) 
VIBR .0, 0.00500 = C(21) TO C(19) 
VIBR .0, 0.00200 = C(21) TO C(22) 
VIBR .0, 0.00500 = C(22) TO C(20) 
VIBR .0, 0.00500 = C(21) TO C(17) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = O(2) TO B(3) 
U(IJ) .0, 0.08000 = B(3) TO O(4) 
U(IJ) .0, 0.08000 = B(3) TO O(5) 
U(IJ) .0, 0.04000 = B(3) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(6) TO C(11) 
U(IJ) .0, 0.04000 = C(7) TO C(8) 
U(IJ) .0, 0.04000 = C(8) TO C(9) 
U(IJ) .0, 0.04000 = C(9) TO C(10) 
U(IJ) .0, 0.04000 = C(10) TO C(11) 
U(IJ) .0, 0.08000 = O(13) TO B(14) 
U(IJ) .0, 0.08000 = B(14) TO O(15) 
U(IJ) .0, 0.08000 = B(14) TO O(16) 
U(IJ) .0, 0.04000 = B(14) TO C(17) 
U(IJ) .0, 0.04000 = C(17) TO C(18) 
U(IJ) .0, 0.04000 = C(17) TO C(22) 
U(IJ) .0, 0.04000 = C(18) TO C(19) 
U(IJ) .0, 0.04000 = C(19) TO C(20) 
U(IJ) .0, 0.04000 = C(20) TO C(21) 
U(IJ) .0, 0.04000 = C(21) TO C(22) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;