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_1551214
_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         'C38 H68 B2 Ca N13 O3 P3, C6 H18 N3 O P'
_chemical_formula_sum            'C44 H86 B2 Ca N16 O4 P4'
_chemical_formula_weight         1088.86
_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                 106.430(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1723(9)
_cell_length_b                   14.0207(5)
_cell_length_c                   20.0498(8)
_cell_measurement_reflns_used    16833
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.0260
_cell_measurement_theta_min      3.7980
_cell_volume                     5978.4(4)
_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    '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 0.995
_diffrn_measured_fraction_theta_max 0.991
_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    -95.00 -13.00   0.50   14.00    --   -5.70   0.00  90.00  164
  2  \w    -33.00   7.00   0.50   14.00    --   -5.70 -82.00-120.00   80
  3  \w    -33.00  23.00   0.50   14.00    --   -5.70 -82.00  60.00  112
  4  \w     29.00  80.00   0.50   14.00    --   -5.70   0.00  90.00  102
  5  \w      5.00  30.00   0.50   14.00    --   -5.70 -77.00-180.00   50
  6  \w    -18.00   8.00   0.50   14.00    --    6.00 -82.00-180.00   52
  7  \w    -46.00  27.00   0.50   14.00    --    6.00 -77.00 120.00  146
;
_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      0.0090946000
_diffrn_orient_matrix_UB_12      0.0476946000
_diffrn_orient_matrix_UB_13      -0.0037637000
_diffrn_orient_matrix_UB_21      0.0294437000
_diffrn_orient_matrix_UB_22      -0.0085224000
_diffrn_orient_matrix_UB_23      0.0247712000
_diffrn_orient_matrix_UB_31      0.0127921000
_diffrn_orient_matrix_UB_32      -0.0144391000
_diffrn_orient_matrix_UB_33      -0.0270929000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66463
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.477
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65629
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         13570
_refine_ls_number_restraints     606
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+11.2799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10683
_reflns_number_total             13570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02118c2.cif
_cod_data_source_block           3a-HMPA
_cod_depositor_comments
'Adding full bibliography for 1551209--1551214.cif.'
_cod_database_code               1551214
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H B N Ca O'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.974
_reflns_odcompleteness_completeness 99.11
_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 N(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
C11 \\sim C4 \\sim C5 \\sim C17 \\sim C16 \\sim C6 \\sim C12 \\sim C15 \\sim C1
\\sim C20 \\sim C14 \\sim C13 \\sim C18 \\sim C3 \\sim C10 \\sim C19 \\sim C2
\\sim C015 \\sim C016 \\sim C017 \\sim C018 \\sim C019 \\sim C9 \\sim C01C
\\sim C7 \\sim C01E \\sim C01F \\sim C8 \\sim C01I \\sim C01J \\sim C01K \\sim
C01L \\sim C01O \\sim C01P \\sim C01S \\sim C01T \\sim C5BA \\sim C22 \\sim
C1BA \\sim C2BA \\sim C3BA \\sim C0AA \\sim C4BA \\sim C6BA \\sim C1AA \\sim
C3AA \\sim C2AA \\sim C4AA \\sim C7BA \\sim C8AA \\sim C5AA \\sim C9AA \\sim
C0BA \\sim C6AA \\sim C7AA \\sim N3 \\sim N1 \\sim N4 \\sim N2 \\sim N11 \\sim
N8 \\sim N00M \\sim N00N \\sim N10 \\sim N012 \\sim N9 \\sim N014 \\sim N01H
\\sim N5A \\sim N5AA \\sim N3AA \\sim N5B \\sim N6 \\sim N7 \\sim N12 \\sim N13
\\sim N2AA: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Hd)=Sof(He)=Sof(Hf)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(H22c)=Sof(N5AA)=
 Sof(N3AA)=Sof(N5B)=Sof(C1BA)=Sof(H1Ba)=Sof(H1Bb)=Sof(H1Bc)=Sof(C4BA)=Sof(H4Ba)=
 Sof(H4Bb)=Sof(H4Bc)=Sof(C1AA)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(C3AA)=
 Sof(H3Aa)=Sof(H3Ab)=Sof(H3Ac)=Sof(C2AA)=Sof(H2Aa)=Sof(H2Ab)=Sof(H2Ac)=
 Sof(C8AA)=Sof(H8Aa)=Sof(H8Ab)=Sof(H8Ac)=Sof(C5AA)=Sof(H5Aa)=Sof(H5Ab)=
 Sof(H5Ac)=Sof(N12)=Sof(C9AA)=Sof(H9Aa)=Sof(H9Ab)=Sof(H9Ac)=Sof(N13)=Sof(C0BA)=
 Sof(H0Ba)=Sof(H0Bb)=Sof(H0Bc)=Sof(N2AA)=Sof(C7AA)=Sof(H7Ab)=Sof(H7Ac)=
 Sof(H7Ad)=1-FVAR(1)
 Sof(N012)=Sof(N014)=Sof(H7aa)=Sof(Hb)=Sof(Hc)=Sof(C01F)=Sof(H01m)=Sof(H01n)=
 Sof(H01o)=Sof(N01H)=Sof(C01L)=Sof(H1ca)=Sof(Hm)=Sof(Hn)=Sof(C01S)=Sof(H01y)=
 Sof(Ho)=Sof(Hp)=Sof(C5BA)=Sof(H5Ba)=Sof(H5Bb)=Sof(H5Bc)=Sof(N5A)=Sof(N6)=
 Sof(N7)=Sof(C2BA)=Sof(H2Ba)=Sof(H2Bb)=Sof(H2Bc)=Sof(C3BA)=Sof(H3Ba)=Sof(H3Bb)=
 Sof(H3Bc)=Sof(C0AA)=Sof(H0Aa)=Sof(H0Ab)=Sof(H0Ac)=Sof(C6BA)=Sof(H6Ba)=
 Sof(H6Bb)=Sof(H6Bc)=Sof(C4AA)=Sof(H4Aa)=Sof(H4Ab)=Sof(H4Ac)=Sof(C7BA)=
 Sof(H7Ba)=Sof(H7Bb)=Sof(H7Bc)=Sof(C6AA)=Sof(H6Aa)=Sof(H6Ab)=Sof(H6Ac)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C12(H12), C1(H1a), C20(H20), C14(H14), C13(H13), C18(H18),
 C3(H3), C19(H19), C2(H2), C9(H9), C7(H7), C8(H8)
4.b Idealised Me refined as rotating group:
 C015(H01a,H01b,H01c), C016(H01,H,Ha), C017(H01d,H01e,H01f), C018(H7aa,Hb,Hc),
 C018(Hd,He,Hf), C019(H01g,H01h,H01i), C01C(H01j,H01k,H01l), C01E(H8ba,Hg,Hh),
 C01F(H01m,H01n,H01o), C01I(H9ba,Hi,Hj), C01J(H01p,H01q,H01r), C01K(H0ca,Hk,Hl),
  C01L(H1ca,Hm,Hn), C01O(H01s,H01t,H01u), C01P(H01v,H01w,H01x), C01S(H01y,Ho,
 Hp), C01T(H01z,Hq,Hr), C5BA(H5Ba,H5Bb,H5Bc), C22(H22a,H22b,H22c), C1BA(H1Ba,
 H1Bb,H1Bc), C2BA(H2Ba,H2Bb,H2Bc), C3BA(H3Ba,H3Bb,H3Bc), C0AA(H0Aa,H0Ab,H0Ac),
 C4BA(H4Ba,H4Bb,H4Bc), C6BA(H6Ba,H6Bb,H6Bc), C1AA(H1Aa,H1Ab,H1Ac), C3AA(H3Aa,
 H3Ab,H3Ac), C2AA(H2Aa,H2Ab,H2Ac), C4AA(H4Aa,H4Ab,H4Ac), C7BA(H7Ba,H7Bb,H7Bc),
 C8AA(H8Aa,H8Ab,H8Ac), C5AA(H5Aa,H5Ab,H5Ac), C9AA(H9Aa,H9Ab,H9Ac), C0BA(H0Ba,
 H0Bb,H0Bc), C6AA(H6Aa,H6Ab,H6Ac), C7AA(H7Ab,H7Ac,H7Ad)
;
_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 2.022
_oxdiff_exptl_absorpt_empirical_full_min 0.626