#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:49:04 +0200 (Thu, 07 Nov 2019) $
#$Revision: 224111 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/96/7049611.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7049611
loop_
_publ_author_name
'Jones, Dafydd D. L.'
'Matthews, Aidan J. R.'
'Jones, Cameron'
_publ_section_title
;
 The complex reactivity of β-diketiminato magnesium(i) dimers towards
 pinacolborane: implications for catalysis.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5785
_journal_page_last               5792
_journal_paper_doi               10.1039/c9dt01085h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C54 H74 B2 Mg2 N4 O6'
_chemical_formula_weight         945.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-04-04 deposited with the CCDC.    2019-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7772(2)
_cell_length_b                   13.77780(10)
_cell_length_c                   20.9610(2)
_cell_measurement_reflns_used    19662
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      77.1950
_cell_measurement_theta_min      3.1780
_cell_volume                     5422.79(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    xseed
_computing_publication_material  Ciftab
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.498
_diffrn_reflns_theta_min         6.329
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0484
_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/[σ²(Fo²)+(0.0638P)²+3.3157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4727
_reflns_number_total             4988
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01085h2.cif
_cod_data_source_block           Cj1346
_cod_depositor_comments
'Adding full bibliography for 7049610--7049618.cif.'
_cod_database_code               7049611
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.891
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mg1 Mg 0.53370(3) 0.57259(4) 0.45725(2) 0.02484(16) Uani 1 1 d . .
O1 O 0.55454(7) 0.50691(9) 0.53809(6) 0.0316(3) Uani 1 1 d . .
N1 N 0.52492(8) 0.71896(10) 0.45663(6) 0.0269(3) Uani 1 1 d . .
C1 C 0.69731(11) 0.55453(14) 0.64499(9) 0.0365(4) Uani 1 1 d . .
B1 B 0.60357(11) 0.50751(15) 0.58306(10) 0.0293(4) Uani 1 1 d . .
O2 O 0.59636(7) 0.45489(9) 0.63956(6) 0.0338(3) Uani 1 1 d . .
N2 N 0.59602(8) 0.56717(10) 0.37816(7) 0.0266(3) Uani 1 1 d . .
C2 C 0.77771(12) 0.55560(19) 0.63928(13) 0.0538(6) Uani 1 1 d . .
H2A H 0.793245 0.500601 0.613100 0.081 Uiso 1 1 calc R U
H2B H 0.798971 0.550519 0.681847 0.081 Uiso 1 1 calc R U
H2C H 0.792950 0.616383 0.619192 0.081 Uiso 1 1 calc R U
O3 O 0.66703(7) 0.55794(10) 0.58095(6) 0.0360(3) Uani 1 1 d . .
C3 C 0.67171(13) 0.64526(15) 0.67935(10) 0.0449(5) Uani 1 1 d . .
H3A H 0.685421 0.702824 0.654786 0.067 Uiso 1 1 calc R U
H3B H 0.693444 0.648283 0.721810 0.067 Uiso 1 1 calc R U
H3C H 0.619754 0.643152 0.683599 0.067 Uiso 1 1 calc R U
C4 C 0.66389(11) 0.46000(14) 0.67260(9) 0.0363(4) Uani 1 1 d . .
C5 C 0.65044(14) 0.46120(17) 0.74372(10) 0.0488(5) Uani 1 1 d . .
H5A H 0.619397 0.516010 0.754416 0.073 Uiso 1 1 calc R U
H5B H 0.695829 0.467943 0.766367 0.073 Uiso 1 1 calc R U
H5C H 0.627374 0.400409 0.756467 0.073 Uiso 1 1 calc R U
C6 C 0.70500(12) 0.36853(15) 0.65434(11) 0.0461(5) Uani 1 1 d . .
H6A H 0.676497 0.311142 0.664874 0.069 Uiso 1 1 calc R U
H6B H 0.750002 0.366446 0.677979 0.069 Uiso 1 1 calc R U
H6C H 0.714897 0.369276 0.608433 0.069 Uiso 1 1 calc R U
C7 C 0.64226(10) 0.48675(14) 0.36432(8) 0.0318(4) Uani 1 1 d . .
C8 C 0.61807(12) 0.40717(15) 0.32950(10) 0.0419(5) Uani 1 1 d . .
C9 C 0.54275(13) 0.40029(18) 0.30663(13) 0.0551(6) Uani 1 1 d . .
H9A H 0.513522 0.368712 0.339329 0.083 Uiso 1 1 calc R U
H9B H 0.541132 0.362053 0.267231 0.083 Uiso 1 1 calc R U
H9C H 0.524268 0.465606 0.298341 0.083 Uiso 1 1 calc R U
C10 C 0.66654(16) 0.33158(17) 0.31682(12) 0.0593(7) Uani 1 1 d . .
H10 H 0.651642 0.277429 0.292137 0.071 Uiso 1 1 calc R U
C11 C 0.73524(15) 0.3351(2) 0.33971(13) 0.0648(8) Uani 1 1 d . .
H11 H 0.767278 0.283535 0.330752 0.078 Uiso 1 1 calc R U
C12 C 0.75742(13) 0.4121(2) 0.37509(12) 0.0583(7) Uani 1 1 d . .
H12 H 0.804730 0.413067 0.391135 0.070 Uiso 1 1 calc R U
C13 C 0.71222(10) 0.48960(17) 0.38826(9) 0.0418(5) Uani 1 1 d . .
C14 C 0.73795(11) 0.5740(2) 0.42660(11) 0.0538(6) Uani 1 1 d . .
H14A H 0.788244 0.564601 0.437448 0.081 Uiso 1 1 calc R U
H14B H 0.709859 0.579107 0.465862 0.081 Uiso 1 1 calc R U
H14C H 0.732623 0.633721 0.401640 0.081 Uiso 1 1 calc R U
C15 C 0.59257(9) 0.63892(13) 0.33564(8) 0.0284(4) Uani 1 1 d . .
C16 C 0.63011(11) 0.62714(15) 0.27232(8) 0.0370(4) Uani 1 1 d . .
H16A H 0.681581 0.622512 0.279430 0.055 Uiso 1 1 calc R U
H16B H 0.619860 0.683345 0.245178 0.055 Uiso 1 1 calc R U
H16C H 0.613221 0.567920 0.251299 0.055 Uiso 1 1 calc R U
C17 C 0.55797(10) 0.72771(13) 0.34544(8) 0.0331(4) Uani 1 1 d . .
H17 H 0.551388 0.766220 0.308306 0.040 Uiso 1 1 calc R U
C18 C 0.53156(10) 0.76804(13) 0.40231(8) 0.0312(4) Uani 1 1 d . .
C19 C 0.51236(13) 0.87481(14) 0.40065(10) 0.0443(5) Uani 1 1 d . .
H19A H 0.464558 0.883897 0.418434 0.066 Uiso 1 1 calc R U
H19B H 0.513236 0.897931 0.356447 0.066 Uiso 1 1 calc R U
H19C H 0.546881 0.911665 0.426011 0.066 Uiso 1 1 calc R U
C20 C 0.51230(10) 0.77205(12) 0.51431(8) 0.0283(4) Uani 1 1 d . .
C21 C 0.44344(10) 0.78047(13) 0.53937(9) 0.0333(4) Uani 1 1 d . .
C22 C 0.38012(11) 0.73730(17) 0.50547(11) 0.0452(5) Uani 1 1 d . .
H22A H 0.380330 0.666667 0.510957 0.068 Uiso 1 1 calc R U
H22B H 0.382683 0.753005 0.459928 0.068 Uiso 1 1 calc R U
H22C H 0.336180 0.764174 0.523487 0.068 Uiso 1 1 calc R U
C23 C 0.43464(11) 0.82986(14) 0.59697(9) 0.0384(4) Uani 1 1 d . .
H23 H 0.388204 0.836880 0.614357 0.046 Uiso 1 1 calc R U
C24 C 0.49196(12) 0.86863(14) 0.62912(9) 0.0393(5) Uani 1 1 d . .
H24 H 0.484919 0.901841 0.668334 0.047 Uiso 1 1 calc R U
C25 C 0.55962(12) 0.85913(14) 0.60423(9) 0.0385(4) Uani 1 1 d . .
H25 H 0.598957 0.885929 0.626639 0.046 Uiso 1 1 calc R U
C26 C 0.57118(10) 0.81081(13) 0.54671(8) 0.0327(4) Uani 1 1 d . .
C27 C 0.64550(11) 0.79936(16) 0.52078(10) 0.0418(5) Uani 1 1 d . .
H27A H 0.678350 0.840000 0.545401 0.063 Uiso 1 1 calc R U
H27B H 0.646425 0.819376 0.475921 0.063 Uiso 1 1 calc R U
H27C H 0.660081 0.731257 0.524135 0.063 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Mg1 O1 82.51(6) . 5_666
O1 Mg1 N1 118.81(6) . .
O1 Mg1 N1 118.77(6) 5_666 .
O1 Mg1 N2 125.01(6) . .
O1 Mg1 N2 120.00(6) 5_666 .
N1 Mg1 N2 94.49(6) . .
B1 O1 Mg1 139.01(12) . .
B1 O1 Mg1 123.41(12) . 5_666
Mg1 O1 Mg1 97.49(6) . 5_666
C18 N1 C20 118.58(14) . .
C18 N1 Mg1 120.31(12) . .
C20 N1 Mg1 121.11(10) . .
O3 C1 C2 108.39(17) . .
O3 C1 C3 106.62(15) . .
C2 C1 C3 110.15(18) . .
O3 C1 C4 102.23(14) . .
C2 C1 C4 116.06(18) . .
C3 C1 C4 112.59(17) . .
O1 B1 O3 125.70(17) . .
O1 B1 O2 122.42(17) . .
O3 B1 O2 111.88(16) . .
B1 O2 C4 107.21(14) . .
C15 N2 C7 117.80(14) . .
C15 N2 Mg1 119.39(12) . .
C7 N2 Mg1 122.77(11) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
B1 O3 C1 106.91(14) . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
O2 C4 C5 109.03(17) . .
O2 C4 C6 106.45(15) . .
C5 C4 C6 109.92(17) . .
O2 C4 C1 102.48(14) . .
C5 C4 C1 115.12(17) . .
C6 C4 C1 113.17(18) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C8 C7 C13 120.87(18) . .
C8 C7 N2 121.03(17) . .
C13 C7 N2 118.08(18) . .
C7 C8 C10 118.1(2) . .
C7 C8 C9 121.72(18) . .
C10 C8 C9 120.2(2) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 C8 120.9(3) . .
C11 C10 H10 119.6 . .
C8 C10 H10 119.6 . .
C12 C11 C10 120.3(2) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C13 121.3(2) . .
C11 C12 H12 119.3 . .
C13 C12 H12 119.3 . .
C12 C13 C7 118.5(2) . .
C12 C13 C14 120.4(2) . .
C7 C13 C14 121.03(19) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N2 C15 C17 124.94(16) . .
N2 C15 C16 119.01(16) . .
C17 C15 C16 116.03(15) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 C18 129.30(16) . .
C15 C17 H17 115.4 . .
C18 C17 H17 115.4 . .
N1 C18 C17 123.93(16) . .
N1 C18 C19 119.40(16) . .
C17 C18 C19 116.64(16) . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C21 C20 C26 120.96(16) . .
C21 C20 N1 120.76(16) . .
C26 C20 N1 118.19(16) . .
C23 C21 C20 118.30(17) . .
C23 C21 C22 120.45(18) . .
C20 C21 C22 121.25(16) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C24 C23 C21 121.31(18) . .
C24 C23 H23 119.3 . .
C21 C23 H23 119.3 . .
C23 C24 C25 119.85(17) . .
C23 C24 H24 120.1 . .
C25 C24 H24 120.1 . .
C24 C25 C26 121.05(18) . .
C24 C25 H25 119.5 . .
C26 C25 H25 119.5 . .
C25 C26 C20 118.53(18) . .
C25 C26 C27 120.43(17) . .
C20 C26 C27 121.04(16) . .
C26 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C26 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 O1 1.9605(13) .
Mg1 O1 1.9886(14) 5_666
Mg1 N1 2.0234(15) .
Mg1 N2 2.0307(15) .
O1 B1 1.318(2) .
N1 C18 1.330(2) .
N1 C20 1.433(2) .
C1 O3 1.459(2) .
C1 C2 1.515(3) .
C1 C3 1.521(3) .
C1 C4 1.557(3) .
B1 O3 1.380(2) .
B1 O2 1.395(2) .
O2 C4 1.447(2) .
N2 C15 1.333(2) .
N2 C7 1.437(2) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.512(3) .
C4 C6 1.527(3) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.393(3) .
C7 C13 1.407(3) .
C8 C10 1.408(3) .
C8 C9 1.496(3) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.377(4) .
C10 H10 0.9500 .
C11 C12 1.360(4) .
C11 H11 0.9500 .
C12 C13 1.391(3) .
C12 H12 0.9500 .
C13 C14 1.494(4) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C17 1.400(3) .
C15 C16 1.512(2) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 C18 1.406(3) .
C17 H17 0.9500 .
C18 C19 1.515(3) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 C21 1.400(3) .
C20 C26 1.403(3) .
C21 C23 1.396(3) .
C21 C22 1.507(3) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 C24 1.378(3) .
C23 H23 0.9500 .
C24 C25 1.380(3) .
C24 H24 0.9500 .
C25 C26 1.394(3) .
C25 H25 0.9500 .
C26 C27 1.506(3) .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
