Structural and metal-halogen exchange reactivity studies of sodium magnesiate biphenolate complexes.
Yeardley, Callum; Kennedy, Alan R.; Gros, Philippe C.; Touchet, Sabrina; Fairley, Michael; McLellan, Ross; Martínez-Martínez, Antonio J; O'Hara, Charles T; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5257–5263; doi:10.1039/d0dt00904k

data_7703951
_publ_section_title
;
 Structural and metal-halogen exchange reactivity studies of sodium
 magnesiate biphenolate complexes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5257
_journal_page_last               5263
_journal_paper_doi               10.1039/d0dt00904k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C50 H96 Mg N6 Na2 O2'
_chemical_formula_sum            'C50 H96 Mg N6 Na2 O2'
_chemical_formula_weight         883.61
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-04 deposited with the CCDC.	2020-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.040(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9924(3)
_cell_length_b                   14.0108(3)
_cell_length_c                   15.4464(5)
_cell_measurement_reflns_used    10306
_cell_measurement_temperature    123.25(10)
_cell_measurement_theta_max      73.1860
_cell_measurement_theta_min      4.6590
_cell_volume                     2768.71(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      123.25(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0268
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -26.00   72.00   1.0000    1.1950
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  150.0000 98

  2 omega   -4.00   42.00   1.0000    1.1950
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   90.0000 46

  3 omega  -21.00   69.00   1.0000    1.1950
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 90

  4 omega  -13.00   77.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000 -180.0000 90

  5 omega  -13.00   77.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000 -120.0000 90

  6 omega   18.00  113.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000 -180.0000 95

  7 omega   35.00  125.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000   30.0000 90

  8 omega   12.00  129.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000   19.0000  -30.0000 117

  9 omega   26.00  126.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -30.0000 100

 10 omega   39.00  178.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -12.0000   90.0000 139

 11 omega   86.00  178.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000   37.0000 -180.0000 92

 12 omega   40.00   92.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000   30.0000 52

 13 omega   42.00  105.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -30.0000 63

 14 omega   42.00  105.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -150.0000 63

 15 omega   39.00   94.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -150.0000 55

 16 omega   39.00   94.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  150.0000 55

 17 omega   40.00  116.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  120.0000 76

 18 omega   40.00   92.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000  -90.0000 52

 19 omega   78.00  178.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000   30.0000 100

 20 omega   40.00  150.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -91.0000 -150.0000 110

 21 omega   40.00  116.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   30.0000 76

 22 omega   39.00   94.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  -30.0000 55

 23 omega   44.00  134.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000   90.0000 90

 24 omega  -72.00   26.00   1.0000    1.1950
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000  150.0000 98

 25 omega   -4.00   42.00   1.0000    1.1950
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  120.0000 46

 26 omega   35.00  125.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000 -180.0000 90

 27 omega  -13.00   77.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000    0.0000 90

 28 omega   26.00  126.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -120.0000 100

 29 omega   26.00  126.00   1.0000    4.7800
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000   90.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0984039000
_diffrn_orient_matrix_UB_12      0.0367940000
_diffrn_orient_matrix_UB_13      -0.0322520000
_diffrn_orient_matrix_UB_21      -0.0464595000
_diffrn_orient_matrix_UB_22      0.1014220000
_diffrn_orient_matrix_UB_23      -0.0082615000
_diffrn_orient_matrix_UB_31      0.0513927000
_diffrn_orient_matrix_UB_32      0.0211399000
_diffrn_orient_matrix_UB_33      0.0955799000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27167
_diffrn_reflns_point_group_measured_fraction_full 0.795
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.207
_diffrn_reflns_theta_min         4.109
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 2457 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8631
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1328P)^2^+0.4717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.566
_reflns_Friedel_fraction_full    0.589
_reflns_Friedel_fraction_max     0.562
_reflns_number_gt                7768
_reflns_number_total             8631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00904k2.cif
_cod_data_source_block           cy2-221
_cod_depositor_comments
'Adding full bibliography for 7703949--7703951.cif.'
_cod_database_code               7703951
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C47 = C46A-C47A = C45-C46 = C46A-C45A
 1.51 with sigma of 0.01
3. Rigid bond restraints
 C43, C45, C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C43 \\sim C45 \\sim C46 \\sim C47: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(C46) = Uanis(C46A)
Uanis(C47) = Uanis(C47A)
Uanis(C45) = Uanis(C45A)
5. Others
 Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=
 Sof(C45A)=Sof(H45C)=Sof(H45D)=1-FVAR(1)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(H47C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B), C49(H49A,H49B),
  C46A(H46C,H46D), C45A(H45C,H45D)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C),
 C47A(H47D,H47E,H47F)
;
_shelx_res_checksum              55441
_olex2_submission_special_instructions 'No special instructions were received'