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_7703950
_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
'C64 H96 Na4 O8, 2(C0.7 H1.4 O0.2), 0.2(C H2)'
_chemical_formula_sum            'C65.6 H99.2 Na4 O8.4'
_chemical_formula_weight         1114.20
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.33310(10)
_cell_length_b                   13.33310(10)
_cell_length_c                   37.0015(5)
_cell_measurement_reflns_used    16640
_cell_measurement_temperature    123.05(10)
_cell_measurement_theta_max      72.5190
_cell_measurement_theta_min      3.5170
_cell_volume                     6577.81(11)
_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      123.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0268
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega   -4.00   42.00   1.0000    2.3750
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 46

  2 omega   65.00  129.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  167.0000  167.0000 64

  3 omega  -13.00   77.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  120.0000 90

  4 omega   40.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000    0.0000 76

  5 omega   40.00   92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000 -180.0000 52

  6 omega   42.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  120.0000 63

  7 omega   42.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000   60.0000 63

  8 omega  -70.00   30.00   1.0000    2.3750
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000   30.0000 100

  9 omega   26.00  126.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  120.0000 100

 10 omega   26.00  126.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000   30.0000 100

 11 omega   35.00  125.00   1.0000   13.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000  -90.0000 90

 12 omega   86.00  168.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   37.0000 -180.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1054867000
_diffrn_orient_matrix_UB_12      0.0297591000
_diffrn_orient_matrix_UB_13      -0.0131554000
_diffrn_orient_matrix_UB_21      0.0430547000
_diffrn_orient_matrix_UB_22      0.0974127000
_diffrn_orient_matrix_UB_23      -0.0161683000
_diffrn_orient_matrix_UB_31      0.0191438000
_diffrn_orient_matrix_UB_32      -0.0545954000
_diffrn_orient_matrix_UB_33      -0.0360380000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            25584
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.182
_diffrn_reflns_theta_min         5.266
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83042
_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    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 2455 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6448
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0877P)^2^+1.8879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.699
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                6182
_reflns_number_total             6448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00904k2.cif
_cod_data_source_block           amsoa02
_cod_depositor_comments
'Adding full bibliography for 7703949--7703951.cif.'
_cod_original_cell_volume        6577.81(13)
_cod_original_formula_sum        'C65.60 H99.20 Na4 O8.40'
_cod_database_code               7703950
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.73
_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
 C29-C30 = C30-C31 = C31-C32 = C29A-C30A = C30A-C31A = C31A-C32A
 1.53 with sigma of 0.01
 O3-C29 = O3-C32 = O3-C29A = O3-C32A = O4-C28 = O4-C25 = O4-C28A = O4-C25A
 1.43 with sigma of 0.01
 C25-C26 = C26-C27 = C27-C28 = C25A-C26A = C26A-C27A = C27A-C28A
 1.53 with sigma of 0.01
 C1S-C2S = C2S-C3S = C1S-C4S = C2S-C5S = C4S-C5S
 1.53 with sigma of 0.01
 O1S-C4S = O1S-C3S
 1.43 with sigma of 0.01
 C4S-C3S
 2.35 with sigma of 0.02
3. Rigid bond restraints
 O3, C29A, C30A, C31A, C32A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3 \\sim C29A \\sim C30A \\sim C31A \\sim C32A: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.02
O4 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.02
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C27) = Uanis(C27A)
Uanis(C28) = Uanis(C28A)
Uanis(C29) = Uanis(C29A)
Uanis(C30) = Uanis(C30A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
5. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=FVAR(1)
 Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=
 Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=1-FVAR(2)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(2)
 Fixed Sof: O1S(0.2) C2S(0.2) H2SA(0.2) H2SB(0.2) C3S(0.2) H3SA(0.2) H3SB(0.2)
 C4S(0.2) H4SA(0.2) H4SB(0.2) C5S(0.1) H5SA(0.1) H5SB(0.1) C1S(0.1) H1SA(0.1)
 H1SB(0.1)
6.a Riding coordinates:
 C1S(H1SA,H1SB)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C29A(H29C,H29D),
 C30A(H30C,H30D), C31A(H31C,H31D), C32A(H32C,H32D), C25A(H25C,H25D), C26A(H26C,
 H26D), C27A(H27C,H27D), C28A(H28C,H28D), C2S(H2SA,H2SB), C3S(H3SA,H3SB),
 C4S(H4SA,H4SB), C5S(H5SA,H5SB)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10)
6.d 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)
;
_shelx_res_checksum              45727
_olex2_submission_special_instructions 'No special instructions were received'