Boron diamide derivatives containing N-N and N-P molecular fragments.
Major, Christopher J.; Chen, Shi-Ming; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2159–2166; doi:10.1039/d3dt03665k

data_7714862
_publ_section_title
;
 Boron diamide derivatives containing N-N and N-P molecular fragments.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2159
_journal_page_last               2166
_journal_paper_doi               10.1039/d3dt03665k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C52 H72 B2 Cl2 N6 P2, C2 H3 N'
_chemical_formula_sum            'C54 H75 B2 Cl2 N7 P2'
_chemical_formula_weight         976.746
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2023-09-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2023-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.900(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3041(12)
_cell_length_b                   12.6196(11)
_cell_length_c                   33.560(3)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      3.23
_cell_volume                     5581.0(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.9920
_diffrn_measured_fraction_theta_max 0.9920
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.9920
_diffrn_reflns_Laue_measured_fraction_max 0.9920
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            112072
_diffrn_reflns_point_group_measured_fraction_full 0.9920
_diffrn_reflns_point_group_measured_fraction_max 0.9920
_diffrn_reflns_theta_full        24.9994
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.65
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             2090.968
_refine_diff_density_max         0.5014
_refine_diff_density_min         -0.4327
_refine_diff_density_rms         0.0905
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             7.6894
_refine_ls_goodness_of_fit_ref   1.0533
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    116
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0533
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+3.6428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                6916
_reflns_number_total             9722
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03665k2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7714859--7714862.cif.'
_cod_database_code               7714862
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C24(H24), C32(H32), C35(H35), C37(H37), C41(H41), C43(H43), C44(H44)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C14(H14), C18(H18), C19(H19), C21(H21), C26(H26),
 C29(H29), C30(H30), C31(H31), C33(H33), C36(H36), C38(H38), C39(H39), C42(H42),
  C50(H50)
2.c Idealised Me refined as rotating group:
 C40(H40a,H40b,H40c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c), C48(H48a,H48b,
 H48c), C49(H49a,H49b,H49c), C51(H51a,H51b,H51c), C53(H53a,H53b,H53c), C54(H54a,
 H54b,H54c), C55(H55a,H55b,H55c), C56(H56a,H56b,H56c), C57(H57a,H57b,H57c),
 C58(H58a,H58b,H58c), C60(H60a,H60b,H60c), C61(H61a,H61b,H61c), C62(H62a,H62b,
 H62c), C63(H63a,H63b,H63c), C59(H59a,H59b,H59c)
;
_olex2_submission_special_instructions 'No special instructions were received'