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_7059731
_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 Mo4 O28, 4(C24 H20 P), 4(C H4 O), 3(H2 O)'
_chemical_formula_sum            'C152 H122 Mo4 O35 P4'
_chemical_formula_weight         3016.13
_chemical_name_common            (PPh4)4[(MoO2)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                   30.160(4)
_cell_length_b                   30.160(4)
_cell_length_c                   14.716(3)
_cell_measurement_reflns_used    1201
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      0.4
_cell_volume                     13386(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    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.1490
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            120107
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        23.512
_diffrn_reflns_theta_max         23.512
_diffrn_reflns_theta_min         0.955
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       Needle
_exptl_crystal_F_000             6168
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 2634 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         9268
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0745
_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^)+(0.0352P)^2^+75.6144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1694
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.926
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                7337
_reflns_number_total             9268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02413a2.cif
_cod_data_source_block           mo4l4pph4
_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_original_cell_volume        13386(5)
_cod_database_code               7059731
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C69A, C70A, C71A, C74A, C72A, C73A, C69B, C70B, C72B, C71B, C74B, C73B, C63A,
 C68A, C67A, C66A, C65A, C64A, C63B, C67B, C68B, C65B, C64B, C66B, C45, C46,
 C47, C48, C49, C50
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: C63A(0.5) C64A(0.5) H64A(0.5) C65A(0.5) H65A(0.5) C66A(0.5)
 H66A(0.5) C67A(0.5) H67A(0.5) C68A(0.5) H68A(0.5) C65B(0.5) H65B(0.5)
 C64B(0.5) H64B(0.5) C66B(0.5) H66B(0.5) C63B(0.5) C67B(0.5) H67B(0.5)
 C68B(0.5) H68B(0.5) C69A(0.5) C73A(0.5) H73A(0.5) C72A(0.5) H72A(0.5)
 C74A(0.5) H74A(0.5) C71A(0.5) H71A(0.5) C70A(0.5) H70A(0.5) C70B(0.5)
 H70B(0.5) C69B(0.5) C73B(0.5) H73B(0.5) C74B(0.5) H74B(0.5) C71B(0.5)
 H71B(0.5) C72B(0.5) H72B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C10(H10), C11(H11), C16(H16), C17(H17), C20(H20),
 C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C64A(H64A), C65A(H65A), C66A(H66A), C67A(H67A), C68A(H68A),
  C65B(H65B), C64B(H64B), C66B(H66B), C67B(H67B), C68B(H68B), C73A(H73A),
 C72A(H72A), C74A(H74A), C71A(H71A), C70A(H70A), C70B(H70B), C73B(H73B),
 C74B(H74B), C71B(H71B), C72B(H72B)
4.b Fitted hexagon refined as free rotating group:
 C63A(C64A,C65A,C66A,C67A,C68A), C65B(C64B,C66B,C63B,C67B,C68B), C69A(C73A,
 C72A,C74A,C71A,C70A), C70B(C69B,C73B,C74B,C71B,C72B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4705
_shelx_fab_checksum              29923
_olex2_submission_special_instructions 'No special instructions were received'