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_7059733
_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
'4(C24 H20 As), C52 H20 Mo4 O28, 4(H2 O), 3(C H4 O)'
_chemical_formula_sum            'C151 H120 As4 Mo4 O35'
_chemical_formula_weight         3177.90
_chemical_name_common            (AsPh4)4[(MoO2)4(9HL)4].3MeOH.4H2O
_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   mixed
_audit_creation_date             2020-06-18
_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                   30.135(4)
_cell_length_b                   30.135(4)
_cell_length_c                   14.809(3)
_cell_measurement_reflns_used    5561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.7553
_cell_measurement_theta_min      0.8144
_cell_volume                     13448(4)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            228684
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.925
_diffrn_reflns_theta_min         0.956
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       Rod
_exptl_crystal_F_000             6424
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 5759 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         16126
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0539P)^2^+21.3593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                14223
_reflns_number_total             16126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02413a2.cif
_cod_data_source_block           mo4l4asph4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'None' was changed
to 'none' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7059731--7059734.cif.

 Adding full bibliography for 7059731--7059734.cif.
;
_cod_database_code               7059733
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.871
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 C64B, C65B, C66B, C67B, C69B, C68B, C69A, C64A, C65A, C66A, C67A, C70A, C75A,
 C74A, C73A, C72A, C71A, C72B, C71B, C73B, C74B, C75B, C70B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: C65A(0.5) H65A(0.5) C64A(0.5) C69A(0.5) H69A(0.5) C68A(0.5)
 H68A(0.5) C67A(0.5) H67A(0.5) C66A(0.5) H66A(0.5) C64B(0.5) C65B(0.5)
 H65B(0.5) C66B(0.5) H66B(0.5) C67B(0.5) H67B(0.5) C69B(0.5) H69B(0.5)
 C68B(0.5) H68B(0.5) C70B(0.5) C75B(0.5) H75B(0.5) C74B(0.5) H74B(0.5)
 C73B(0.5) H73B(0.5) C72B(0.5) H72B(0.5) C71B(0.5) H71B(0.5) C70A(0.5)
 C75A(0.5) H75A(0.5) C74A(0.5) H74A(0.5) C73A(0.5) H73A(0.5) C72A(0.5)
 H72A(0.5) C71A(0.5) H71A(0.5)
4.a Free rotating group:
 O15(H15A,H15B)
4.b Aromatic/amide H refined with riding coordinates:
 C65A(H65A), C69A(H69A), C68A(H68A), C67A(H67A), C66A(H66A), C65B(H65B),
 C66B(H66B), C67B(H67B), C69B(H69B), C68B(H68B), C75B(H75B), C74B(H74B),
 C73B(H73B), C72B(H72B), C71B(H71B), C75A(H75A), C74A(H74A), C73A(H73A),
 C72A(H72A), C71A(H71A), C42(H42), C3(H3), C4(H4), C7(H7), C53(H53), C10(H10),
 C11(H11), C56(H56), C16(H16), C17(H17), C51(H51), C61(H61), C23(H23), C24(H24),
  C62(H62), C35(H35), C37(H37), C33(H33), C49(H49), C59(H59), C32(H32),
 C41(H41), C57(H57), C44(H44), C47(H47), C60(H60), C48(H48), C39(H39), C30(H30),
  C63(H63), C31(H31), C36(H36), C29(H29), C43(H43), C50(H50), C54(H54),
 C38(H38), C55(H55), C45(H45), C20(H20)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4179
_shelx_fab_checksum              49902
_olex2_submission_special_instructions 'No special instructions were received'