Organophosphorus decorated lithium borate and phosphate salts with extended π-conjugated backbone.
Delgado Rosario, Emalyn; Rectenwald, Michael F.; Gaffen, Joshua R.; Rheingold, Arnold L.; Protasiewicz, John D.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6667–6672; doi:10.1039/d1dt00601k

data_7707257
_publ_section_title
;
 Organophosphorus decorated lithium borate and phosphate salts with
 extended \p-conjugated backbone.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6667
_journal_page_last               6672
_journal_paper_doi               10.1039/d1dt00601k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C72 H96 B2 Li2 O32 P8'
_chemical_formula_sum            'C72 H96 B2 Li2 O32 P8'
_chemical_formula_weight         1756.74
_chemical_name_systematic
'lithium octaethyl (2\l4-2,2'-spirobi[naphtho[2,3-d][1,3,2]dioxaborole]-4,4',9,9'-tetrayl)tetrakis(phosphonate)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-21 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                73.891(5)
_cell_angle_beta                 83.711(4)
_cell_angle_gamma                78.620(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3498(18)
_cell_length_b                   19.335(3)
_cell_length_c                   23.900(4)
_cell_measurement_reflns_used    4483
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.111
_cell_measurement_theta_min      2.232
_cell_volume                     4062.5(12)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_unetI/netI     0.1443
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41961
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.376
_diffrn_reflns_theta_min         0.888
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.4908
_exptl_absorpt_correction_T_min  0.4272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0557 before and 0.0487 after correction. The Ratio of minimum to maximum transmission is 0.8704. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         16584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0567P)^2^+1.4053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8870
_reflns_number_total             16584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00601k2.cif
_cod_data_source_block           p_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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 7707256--7707257.cif.
;
_cod_original_cell_volume        4062.5(13)
_cod_database_code               7707257
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.936
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C19(H19A,H19B), C21(H21A,
 H21B), C23(H23A,H23B), C25(H25A,H25B), C38(H38A,H38B), C40(H40A,H40B),
 C49(H49A,H49B), C51(H51A,H51B), C54(H54A,H54B), C65(H65A,H65B), C67(H67A,H67B),
  C70(H70A,H70B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C32(H32), C34(H34), C35(H35),
 C36(H36), C43(H43), C44(H44), C45(H45), C46(H46), C58(H58), C59(H59), C60(H60),
  C61(H61)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C),
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,
 H69B,H69C)
;
_shelx_res_checksum              35378
_shelx_hkl_checksum              24056
_olex2_submission_special_instructions 'No special instructions were received'