Super electron donors derived from diboron.
Zhang, Li; Jiao, Lei; Chemical science 9 (2018) 2711–2722; doi:10.1039/c8sc00008e

data_1548905
_publ_section_title
;
 Super electron donors derived from diboron.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2711
_journal_page_last               2722
_journal_paper_doi               10.1039/c8sc00008e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety
'0.25(C64 H78 B2 K2 N4 O8), 0.25(C64 H73 B2 K2 N4 O8)'
_chemical_formula_sum            'C32 H38 B K N2 O4'
_chemical_formula_weight         564.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1q78x4
_audit_creation_date             2017-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-11-16 deposited with the CCDC.
2018-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.798(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3892(10)
_cell_length_b                   40.276(5)
_cell_length_c                   12.9956(7)
_cell_measurement_reflns_used    2855
_cell_measurement_temperature    175(1)
_cell_measurement_theta_max      66.2700
_cell_measurement_theta_min      4.7160
_cell_volume                     6484.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      175(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.817
_diffrn_measured_fraction_theta_max 0.786
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -11.00  29.00   1.00   13.95    --  -40.81  38.00 -30.00   40
  2  \w    -94.00 -34.00   1.00   13.95    --  -40.81 125.00-150.00   60
  3  \w   -112.00 -43.00   1.00   13.95    --  -40.81 -57.00  60.00   69
  4  \w     29.00 113.00   1.00   55.77    --  100.91-125.00-120.00   84
  5  \w     20.00 151.00   1.00   55.77    --  100.91   0.00  30.00  131
  6  \w    119.00 145.00   1.00   55.77    --  100.91 117.00-113.00   26
  7  \w    129.00 156.00   1.00   55.77    --  100.91 125.00-150.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0428498000
_diffrn_orient_matrix_UB_12      0.0346683000
_diffrn_orient_matrix_UB_13      0.0280656000
_diffrn_orient_matrix_UB_21      0.1114733000
_diffrn_orient_matrix_UB_22      0.0150808000
_diffrn_orient_matrix_UB_23      -0.0227354000
_diffrn_orient_matrix_UB_31      -0.0348340000
_diffrn_orient_matrix_UB_32      0.0055926000
_diffrn_orient_matrix_UB_33      -0.1129967000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0889
_diffrn_reflns_Laue_measured_fraction_full 0.817
_diffrn_reflns_Laue_measured_fraction_max 0.786
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17216
_diffrn_reflns_point_group_measured_fraction_full 0.566
_diffrn_reflns_point_group_measured_fraction_max 0.542
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.496
_diffrn_reflns_theta_min         3.568
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       needle
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 1704 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.437(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1465
_refine_ls_number_reflns         13676
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0829P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1833
_reflns_Friedel_coverage         0.358
_reflns_Friedel_fraction_full    0.307
_reflns_Friedel_fraction_max     0.290
_reflns_number_gt                8960
_reflns_number_total             13676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00008e2.cif
_cod_data_source_block           'global_CCDC1'
_cod_depositor_comments
'Adding full bibliography for 1548904--1548905.cif.'
_cod_original_cell_volume        6483.9(10)
_cod_database_code               1548905
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 83.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 Ternary CH refined with riding coordinates:
 C00Q(H00Q), C013(H013), C014(H014), C016(H016), C01D(H01N), C01F(H01Q),
 C01V(H01V), C021(H021), C027(H027), C02P(H02R), C033(H033), C036(H036),
 C03M(H6AA)
2.b Secondary CH2 refined with riding coordinates:
 C049(H04D,H04E), C04C(H04F,H04G)
2.c Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00U(H00U), C00Z(H00Z), C011(H011), C018(H018), C01A(H01A),
 C01E(H01P), C01O(H01O), C01Q(H01S), C01R(H01R), C01U(H01X), C01Y(H01Y),
 C020(H020), C024(H024), C026(H026), C028(H028), C029(H029), C02E(H02E),
 C02J(H02J), C02K(H1AA), C02Q(H02S), C02R(H02T), C02S(H02U), C02T(H3AA),
 C02V(H02V), C02W(H02W), C02X(H02X), C030(H030), C031(H031), C034(H034),
 C035(H035), C038(H038), C039(H039), C03A(H03A), C03B(H03O), C03D(H03P),
 C03E(H03Q), C03G(H03G), C03H(H03H), C03I(H03I), C03J(H03Y), C03K(H03),
 C03L(H5AA), C03N(H03N), C03Q(H7AA), C03R(H03R), C03S(H03S), C03U(H03U),
 C03V(H8AA), C03X(H03X), C03Y(H9AA), C03Z(H03Z), C040(H040), C041(H041),
 C042(H042), C043(H043), C044(H044), C047(H047), C048(H048), C04A(H04O),
 C04B(H04P), C04D(H04H)
2.d Idealised Me refined as rotating group:
 C01B(H01K,H01L,H01M), C01N(H01B,H01C,H01D), C01P(H01E,H01F,H01G), C01S(H01T,
 H01U,H01W), C01W(H01H,H01I,H01J), C022(H02A,H02B,H02C), C023(H02Y,H,HA),
 C02A(H02Z,HB,HC), C02C(H02,HD,HE), C02F(H02D,H02F,H02G), C02H(H0AA,HF,HG),
 C02L(H02H,H02I,H02K), C02M(H02L,H02M,H02N), C02N(H2AA,HH,HI), C02O(H02O,H02P,
 H02Q), C02U(H4AA,HJ,HK), C032(H03K,H03L,H03M), C03F(H03T,H03V,H03W), C03T(H03B,
 H03C,H03D), C03W(H03E,H03F,H03J), C045(H04L,H04M,H04N), C046(H04A,H04B,H04C),
 C04E(H04I,H04J,H04K), C04H(H04Q,H04R,H04S)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.519
_oxdiff_exptl_absorpt_empirical_full_min 0.627