Alkaline-earth metallacyclic complexes bearing a diborane-bridged tetraamide ligand: synthesis, structure and fluorescence property.
Li, Nan; Zhao, Zifeng; Yu, Chao; Wu, Botao; Bian, Zuqiang; Zhang, Wen-Xiong; Xi, Zhenfeng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9067–9071; doi:10.1039/c9dt02118c

data_1551212
_publ_section_title
;
 Alkaline-earth metallacyclic complexes bearing a diborane-bridged
 tetraamide ligand: synthesis, structure and fluorescence property.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9067
_journal_page_last               9071
_journal_paper_doi               10.1039/c9dt02118c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H38 B2 Mg N4 O3, 2(C4 H8 O)'
_chemical_formula_sum            'C40 H54 B2 Mg N4 O5'
_chemical_formula_weight         716.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     iterative
_audit_creation_date             2019-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-28 deposited with the CCDC.    2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.772(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2144(11)
_cell_length_b                   29.474(3)
_cell_length_c                   11.6873(11)
_cell_measurement_reflns_used    14897
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.7220
_cell_measurement_theta_min      2.2370
_cell_volume                     3781.8(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -46.00 -20.00   0.50    3.00    --  -15.70  77.00 150.00   52
  2  \w    -56.00 -30.00   0.50    3.00    --  -15.70  77.00 -90.00   52
  3  \w    -33.00  -7.00   0.50    3.00    --  -15.70 -77.00 150.00   52
  4  \w    -34.00  45.00   0.50    3.00    --   15.80 -82.00-150.00  158
  5  \w    -31.00  60.00   0.50    3.00    --   15.80 -82.00-180.00  182
  6  \w    -29.00  60.00   0.50    3.00    --   15.80 -82.00 -60.00  178
  7  \w    -59.00  33.00   0.50    3.00    --   15.80 -59.00  88.00  184
  8  \w    -41.00  46.00   0.50    3.00    --   15.80 -77.00  60.00  174
  9  \w    -35.00  -9.00   0.50    3.00    --   15.80 -57.00   0.00   52
 10  \w     -5.00  21.00   0.50    3.00    --   15.80 -57.00   0.00   52
 11  \w     34.00  59.00   0.50    3.00    --   15.80 -82.00  60.00   50
 12  \w    -38.00  53.00   0.50    3.00    --   15.80 -77.00 -30.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0041458000
_diffrn_orient_matrix_UB_12      -0.0156859000
_diffrn_orient_matrix_UB_13      -0.0450381000
_diffrn_orient_matrix_UB_21      0.0617143000
_diffrn_orient_matrix_UB_22      0.0062094000
_diffrn_orient_matrix_UB_23      0.0034647000
_diffrn_orient_matrix_UB_31      0.0186374000
_diffrn_orient_matrix_UB_32      -0.0172324000
_diffrn_orient_matrix_UB_33      0.0422799000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            53589
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.909
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+2.9518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7134
_reflns_number_total             8653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02118c2.cif
_cod_data_source_block           2a-2THF
_cod_depositor_comments
'Adding full bibliography for 1551209--1551214.cif.'
_cod_database_code               1551212
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H B N O Mg'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.990
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00S(H00a,H00b), C00V(H00c,H00d), C00Z(H00e,H00f), C01D(H01a,H01b), C010(H01c,
 H01d), C012(H01e,H01f), C013(H01g,H01h), C014(H01i,H01j), C015(H01k,H01l),
 C016(H01m,H01n), C018(H01o,H01p), C019(H01q,H01r), C00Y(H00g,H00h), C01C(H01s,
 H01t), C01E(H01u,H01v), C017(H01w,H01x), C01A(H01y,H), C01B(H01z,Ha), C01F(H01,
 Hb), C01G(H0aa,Hc)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C9(H9), C7(H7), C8(H8), C1(H1a), C18(H18), C3(H3), C2(H2),
 C19(H19), C20(H20), C12(H12), C14(H14), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.578
_oxdiff_exptl_absorpt_empirical_full_min 0.676