A new fluorone-based bridging ligand for discrete and polymeric assemblies including Mo and W based [4+4] metallocycles
Sutton, Ashley L.; Abrahams, Brendan F.; Hudson, Timothy A.; Robson, Richard; New Journal of Chemistry 44 (2020) 11437–11440; doi:10.1039/D0NJ02413A

data_7059732
_publ_section_title
;
 A new fluorone-based bridging ligand for discrete and polymeric
 assemblies including Mo and W based [4+4] metallocycles
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11437
_journal_page_last               11440
_journal_paper_doi               10.1039/D0NJ02413A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'C52 H20 O28 W4, 4(C24 H20 As), 4(C H4 O), 4(H2 0)'
_chemical_formula_sum            'C152 H124 As4 O36 W4'
_chemical_formula_weight         3561.58
_chemical_name_common            (AsPh4)4[(WO2)4(9HL)4].4MeOH.4H2O
_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   geom
_audit_creation_date             2020-06-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-21 deposited with the CCDC.	2020-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.3905(3)
_cell_length_b                   30.3905(3)
_cell_length_c                   14.8757(2)
_cell_measurement_reflns_used    13590
_cell_measurement_temperature    130.15
_cell_measurement_theta_max      4.0840
_cell_measurement_theta_min      73.6780
_cell_volume                     13738.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            27926
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.496
_diffrn_reflns_theta_max         67.496
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.775
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       Rod
_exptl_crystal_F_000             7008
_exptl_crystal_size_max          0.2154
_exptl_crystal_size_mid          0.0782
_exptl_crystal_size_min          0.0637
_refine_diff_density_max         2.308
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 4665 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         12316
_refine_ls_number_restraints     267
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+67.5251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                11498
_reflns_number_total             12316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02413a2.cif
_cod_data_source_block           wl4asph4
_cod_depositor_comments
;Adding full bibliography for 7059731--7059734.cif.

 Adding full bibliography for 7059731--7059734.cif.
;
_cod_database_code               7059732
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid body (RIGU) restrains
 O9, C15, C17, C19, C20, C22, C23, C26, O12, O13, C25, C24, C21, O11, C18, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C69B, C74B, C73B, C72B, C71B, C70B, C69A, C74A, C73A, C72A, C71A, C70A, C63A,
 C64A, C65A, C66A, C67A, C68A, C64B, C65B, C66B, C67B, C68B, C63B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: C68A(0.5) H68A(0.5) C67A(0.5) H67A(0.5) C66A(0.5) H66A(0.5)
 C65A(0.5) H65A(0.5) C64A(0.5) H64A(0.5) C63A(0.5) C64B(0.5) H64B(0.5)
 C65B(0.5) H65B(0.5) C66B(0.5) H66B(0.5) C67B(0.5) H67B(0.5) C68B(0.5)
 H68B(0.5) C63B(0.5) C69A(0.5) C70A(0.5) H70A(0.5) C72A(0.5) H72A(0.5)
 C71A(0.5) H71A(0.5) C73A(0.5) H73A(0.5) C74A(0.5) H74A(0.5) C71B(0.5)
 H71B(0.5) C74B(0.5) H74B(0.5) C73B(0.5) H73B(0.5) C72B(0.5) H72B(0.5)
 C70B(0.5) H70B(0.5) C69B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C11(H11), C16(H16), C34(H34), C38(H38), C40(H40), C41(H41),
 C43(H43), C55(H55), C7(H7), C10(H10), C17(H17), C20(H20), C23(H23), C24(H24),
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C46(H46),
  C47(H47), C48(H48), C52(H52), C53(H53), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C54(H54), C56(H56), C42(H42), C44(H44), C49(H49), C50(H50),
  C37(H37), C68A(H68A), C67A(H67A), C66A(H66A), C65A(H65A), C64A(H64A),
 C64B(H64B), C65B(H65B), C66B(H66B), C67B(H67B), C68B(H68B), C70A(H70A),
 C72A(H72A), C71A(H71A), C73A(H73A), C74A(H74A), C71B(H71B), C74B(H74B),
 C73B(H73B), C72B(H72B), C70B(H70B)
4.b Fitted hexagon refined as free rotating group:
 C68A(C67A,C66A,C65A,C64A,C63A), C64B(C65B,C66B,C67B,C68B,C63B)
4.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C)
4.d Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91346
_shelx_fab_checksum              5930
_olex2_submission_special_instructions 'No special instructions were received'