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_1551213
_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         'C56 H120 B2 N22 O6 P6 Sr2'
_chemical_formula_sum            'C56 H120 B2 N22 O6 P6 Sr2'
_chemical_formula_weight         1580.41
_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
_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                 99.702(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3034(2)
_cell_length_b                   23.7498(4)
_cell_length_c                   23.2747(4)
_cell_measurement_reflns_used    24998
_cell_measurement_temperature    99.8(5)
_cell_measurement_theta_max      29.2350
_cell_measurement_theta_min      2.0130
_cell_volume                     7793.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(5)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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    -56.00 -30.00   0.50    7.30    --  -15.70  77.00  90.00   52
  2  \w    -31.00  23.00   0.50    7.30    --  -15.70  57.00  30.00  108
  3  \w    -55.00  -9.00   0.50    7.30    --  -15.70  77.00  30.00   92
  4  \w    -59.00 -33.00   0.50    7.30    --  -15.70  80.00 -19.24   52
  5  \w    -32.00  74.00   0.50    7.30    --  -15.70  57.00-120.00  212
  6  \w     47.00  73.00   0.50    7.30    --  -15.70  57.00  30.00   52
  7  \w    -56.00 -29.00   0.50    7.30    --  -15.70  77.00 150.00   54
  8  \w    -54.00  -9.00   0.50    7.30    --  -15.70  77.00-120.00   90
  9  \w     14.00  74.00   0.50    7.30    --  -15.70  57.00 120.00  120
 10  \w    -56.00 -15.00   0.50    7.30    --  -15.70  77.00-180.00   82
 11  \w     19.00 100.00   0.50    7.30    --   15.80  57.00  60.00  162
 12  \w      8.00  57.00   0.50    7.30    --   15.80  70.00 -41.83   98
 13  \w      4.00 105.00   0.50    7.30    --   15.80  57.00 150.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0045347000
_diffrn_orient_matrix_UB_12      0.0196875000
_diffrn_orient_matrix_UB_13      0.0232390000
_diffrn_orient_matrix_UB_21      0.0289386000
_diffrn_orient_matrix_UB_22      0.0172576000
_diffrn_orient_matrix_UB_23      -0.0146466000
_diffrn_orient_matrix_UB_31      -0.0408943000
_diffrn_orient_matrix_UB_32      0.0143811000
_diffrn_orient_matrix_UB_33      -0.0141815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            92785
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.972
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
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    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.459
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         13532
_refine_ls_number_restraints     2118
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+17.5137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10511
_reflns_number_total             13532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02118c2.cif
_cod_data_source_block           4b
_cod_depositor_comments
'Adding full bibliography for 1551209--1551214.cif.'
_cod_database_code               1551213
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.747
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C10 \\sim C5 \\sim C11 \\sim C4 \\sim C16 \\sim C12 \\sim C17 \\sim C9 \\sim C6
\\sim C15 \\sim C3 \\sim C13 \\sim C1 \\sim C92 \\sim C14 \\sim C7 \\sim C2
\\sim C8 \\sim C18 \\sim C19 \\sim C38 \\sim C48 \\sim C44 \\sim C20 \\sim C69
\\sim C46 \\sim C54 \\sim C67 \\sim C0BA \\sim C5BA \\sim C21 \\sim C7BA \\sim
C61 \\sim C1CA \\sim C42 \\sim C3BA \\sim C6BA \\sim C65 \\sim C34 \\sim C71
\\sim C55 \\sim C22 \\sim C68 \\sim C57 \\sim C24 \\sim C45 \\sim C60 \\sim C35
\\sim C51 \\sim C59 \\sim C0CA \\sim C9BA \\sim C1BA \\sim C1AA \\sim C4BA
\\sim C2AA \\sim C3AA \\sim C4AA \\sim C2BA \\sim C0AA \\sim C5AA \\sim C6AA
\\sim C7AA \\sim C8BA \\sim C9AA \\sim C8AA: within 5A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C1BA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(N33)=Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(H34c)=Sof(H1Bd)=Sof(H1Be)=Sof(H1Bf)=
 Sof(C1AA)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(C4BA)=Sof(H4Ba)=Sof(H4Bb)=
 Sof(H4Bc)=Sof(C2AA)=Sof(H2Aa)=Sof(H2Ab)=Sof(H2Ac)=Sof(N3AA)=Sof(C3AA)=
 Sof(H3Aa)=Sof(H3Ab)=Sof(H3Ac)=Sof(C4AA)=Sof(H4Aa)=Sof(H4Ab)=Sof(H4Ac)=
 Sof(N0AA)=Sof(C6AA)=Sof(H6Aa)=Sof(H6Ab)=Sof(H6Ac)=Sof(C7AA)=Sof(H7Aa)=
 Sof(H7Ab)=Sof(H7Ac)=Sof(C9AA)=Sof(H9Aa)=Sof(H9Ab)=Sof(H9Ac)=Sof(C8AA)=
 Sof(H8Aa)=Sof(H8Ab)=Sof(H8Ac)=Sof(Sr1A)=Sof(Sr2A)=1-FVAR(1)
 Sof(Sr2)=Sof(Sr1)=Sof(N25)=Sof(C55)=Sof(H55a)=Sof(H55b)=Sof(H55c)=Sof(C57)=
 Sof(H57a)=Sof(H57b)=Sof(H57c)=Sof(C60)=Sof(H60a)=Sof(H60b)=Sof(H60c)=Sof(C35)=
 Sof(H35a)=Sof(H35b)=Sof(H35c)=Sof(C51)=Sof(H51a)=Sof(H51b)=Sof(H51c)=Sof(C59)=
 Sof(H59a)=Sof(H59b)=Sof(H59c)=Sof(N2AA)=Sof(H1Ba)=Sof(H1Bb)=Sof(H1Bc)=
 Sof(C2BA)=Sof(H2Ba)=Sof(H2Bb)=Sof(H2Bc)=Sof(C0AA)=Sof(H0Aa)=Sof(H0Ab)=
 Sof(H0Ac)=Sof(C5AA)=Sof(H5Aa)=Sof(H5Ab)=Sof(H5Ac)=Sof(N1AA)=Sof(C8BA)=
 Sof(H8Ba)=Sof(H8Bb)=Sof(H8Bc)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C9(H9), C3(H3), C13(H13), C1(H1), C92(H92), C14(H14), C7(H7),
 C2(H2), C8(H8), C18(H18), C19(H19)
4.b Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C48(H48a,H48b,H48c), C44(H44a,H44b,H44c), C20(H20a,H20b,
 H20c), C69(H69a,H69b,H69c), C46(H46a,H46b,H46c), C54(H54a,H54b,H54c), C67(H67a,
 H67b,H67c), C0BA(H0Ba,H0Bb,H0Bc), C5BA(H5Ba,H5Bb,H5Bc), C21(H21a,H21b,H21c),
 C7BA(H7Ba,H7Bb,H7Bc), C61(H61a,H61b,H61c), C1CA(H1Ca,H1Cb,H1Cc), C42(H42a,H42b,
 H42c), C3BA(H3Ba,H3Bb,H3Bc), C6BA(H6Ba,H6Bb,H6Bc), C65(H65a,H65b,H65c),
 C34(H34a,H34b,H34c), C71(H71a,H71b,H71c), C55(H55a,H55b,H55c), C22(H22a,H22b,
 H22c), C68(H68a,H68b,H68c), C57(H57a,H57b,H57c), C24(H24a,H24b,H24c), C45(H45a,
 H45b,H45c), C60(H60a,H60b,H60c), C35(H35a,H35b,H35c), C51(H51a,H51b,H51c),
 C59(H59a,H59b,H59c), C0CA(H0Ca,H0Cb,H0Cc), C9BA(H9Ba,H9Bb,H9Bc), C1BA(H1Ba,
 H1Bb,H1Bc), C1BA(H1Bd,H1Be,H1Bf), C1AA(H1Aa,H1Ab,H1Ac), C4BA(H4Ba,H4Bb,H4Bc),
 C2AA(H2Aa,H2Ab,H2Ac), C3AA(H3Aa,H3Ab,H3Ac), C4AA(H4Aa,H4Ab,H4Ac), C2BA(H2Ba,
 H2Bb,H2Bc), C0AA(H0Aa,H0Ab,H0Ac), C5AA(H5Aa,H5Ab,H5Ac), C6AA(H6Aa,H6Ab,H6Ac),
 C7AA(H7Aa,H7Ab,H7Ac), C8BA(H8Ba,H8Bb,H8Bc), C9AA(H9Aa,H9Ab,H9Ac), C8AA(H8Aa,
 H8Ab,H8Ac)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.746