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_7703949
_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 Mg Na2 O8'
_chemical_formula_sum            'C64 H96 Mg Na2 O8'
_chemical_formula_weight         1063.69
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3684(11)
_cell_length_b                   15.6863(16)
_cell_length_c                   18.5667(12)
_cell_measurement_reflns_used    3415
_cell_measurement_temperature    156(2)
_cell_measurement_theta_max      29.9832
_cell_measurement_theta_min      3.1102
_cell_volume                     3311.0(5)
_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_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_temperature      156.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7323
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.116
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
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    1.067
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 968 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.16(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3269
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0583P)^2^+0.9228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.623
_reflns_Friedel_fraction_full    0.817
_reflns_Friedel_fraction_max     0.789
_reflns_number_gt                2829
_reflns_number_total             3269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00904k2.cif
_cod_data_source_block           amcy04_sq
_cod_depositor_comments
'Adding full bibliography for 7703949--7703951.cif.'
_cod_database_code               7703949
_shelx_shelxl_version_number     2018/3
_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
 O2-C13 = O2-C16 = O2A-C13A = O2A-C16A
 1.43 with sigma of 0.01
 C13-C14 = C14-C15 = C15-C16 = C13A-C14A = C14A-C15A = C15A-C16A
 1.53 with sigma of 0.01
3. Rigid bond restraints
 O2, C13, C14, C15, C16, O2A, C13A, C14A, C15A, C16A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O2 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim O2A \\sim C13A \\sim C14A
\\sim C15A \\sim C16A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(O2) = Uanis(O2A)
Uanis(C13) = Uanis(C13A)
Uanis(C14) = Uanis(C14A)
Uanis(C15) = Uanis(C15A)
Uanis(C16) = Uanis(C16A)
5. Others
 Sof(O2A)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=1-FVAR(1)
 Sof(O2)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=
 Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C13A(H13C,
 H13D), C14A(H14C,H14D), C15A(H15C,H15D), C16A(H16C,H16D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              43516
_shelx_fab_checksum              36903
_olex2_submission_special_instructions 'No special instructions were received'