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_7059734
_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 P), 3(H2 O), 4(C H4 O)'
_chemical_formula_sum            'C152 H122 O35 P4 W4'
_chemical_formula_weight         3367.77
_chemical_name_common            (PPh4)4[(WO2)4(9HL)4].4MeOH.3H2O
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 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                   30.2142(2)
_cell_length_b                   30.2142(2)
_cell_length_c                   14.7473(2)
_cell_measurement_reflns_used    21687
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0960
_cell_measurement_theta_min      2.9110
_cell_volume                     13462.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_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_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47975
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.041
_diffrn_reflns_theta_min         2.925
_exptl_absorpt_coefficient_mu    7.282
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
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    1.662
_exptl_crystal_description       Rod
_exptl_crystal_F_000             6680
_exptl_crystal_size_max          0.538
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.701
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 5129 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         13947
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0540P)^2^+15.0848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                12715
_reflns_number_total             13947
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02413a2.cif
_cod_data_source_block           wl4pph4
_cod_depositor_comments
;Adding full bibliography for 7059731--7059734.cif.

 Adding full bibliography for 7059731--7059734.cif.
;
_cod_original_cell_volume        13462.8(3)
_cod_database_code               7059734
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.622
_shelx_estimated_absorpt_t_min   0.111
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C63A, C64A, C65A, C66A, C67A, C62A, C62B, C63B, C64B, C65B, C66B, C67B, C73B,
 C72B, C71B, C68B, C69B, C71A, C72A, C73A, C68A, C69A, C70A, C70B
 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) C69A(0.5) H69A(0.5) C70A(0.5) H70A(0.5)
 C71A(0.5) H71A(0.5) C72A(0.5) H72A(0.5) C73A(0.5) C62A(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) H63A(0.5) C73B(0.5) H73B(0.5) C69B(0.5) H69B(0.5) C71B(0.5)
 H71B(0.5) C72B(0.5) H72B(0.5) C68B(0.5) C70B(0.5) H70B(0.5) C63B(0.5)
 H63B(0.5) C64B(0.5) H64B(0.5) C62B(0.5) C65B(0.5) H65B(0.5) C67B(0.5)
 H67B(0.5) C66B(0.5) H66B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C20(H20), C59(H59), C24(H24), C17(H17), C60(H60), C4(H4),
 C32(H32), C29(H29), C61(H61), C57(H57), C51(H51), C16(H16), C43(H43), C3(H3),
 C39(H39), C11(H11), C23(H23), C42(H42), C58(H58), C34(H34), C41(H41), C52(H52),
  C35(H35), C47(H47), C31(H31), C53(H53), C28(H28), C49(H49), C36(H36),
 C023(H023), C45(H45), C48(H48), C30(H30), C55(H55), C40(H40), C68A(H68A),
 C69A(H69A), C70A(H70A), C71A(H71A), C72A(H72A), C46(H46), C54(H54), C37(H37),
 C67A(H67A), C66A(H66A), C65A(H65A), C64A(H64A), C63A(H63A), C73B(H73B),
 C69B(H69B), C71B(H71B), C72B(H72B), C70B(H70B), C63B(H63B), C64B(H64B),
 C65B(H65B), C67B(H67B), C66B(H66B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66153
_shelx_fab_checksum              82337
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;