Catalytic hydroboration of carbonyl derivatives by using phosphinimino amide ligated magnesium complexes.
Li, Min; Liu, Xinli; Cui, Dongmei; Dalton transactions (Cambridge, England : 2003) 50 (2021) 13037–13041; doi:10.1039/d1dt00143d

data_7708042
_publ_section_title
;
 Catalytic hydroboration of carbonyl derivatives by using phosphinimino
 amide ligated magnesium complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13037
_journal_page_last               13041
_journal_paper_doi               10.1039/d1dt00143d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C68 H102 Mg2 N4 O2 P2, 1[C7H8], 1[C7H8]'
_chemical_formula_sum            'C82 H118 Mg2 N4 O2 P2'
_chemical_formula_weight         1302.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-07-23
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2021-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7679(4)
_cell_length_b                   28.7777(8)
_cell_length_c                   21.0706(6)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      26.931
_cell_measurement_theta_min      2.303
_cell_volume                     7727.3(4)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            151714
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.116
_diffrn_reflns_theta_min         2.062
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         17057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0438P)^2^+3.4657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12646
_reflns_number_total             17057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00143d2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7708042.cif.'
_cod_database_code               7708042
_shelx_shelxl_version_number     2018/3
_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:
 C12(H12), C18(H18), C22(H22), C28(H28), C30(H30), C58(H58), C70(H70), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C46(H46A,H46B), C48(H48A,H48B), C50(H50A,H50B), C62(H62A,
 H62B), C66(H66A,H66B), C19(H19A,H19B), C45(H45A,H45B), C23(H23A,H23B),
 C47(H47A,H47B), C3(H3A,H3B), C49(H49A,H49B), C13(H13A,H13B), C53(H53A,H53B),
 C27(H27A,H27B), C29(H29A,H29B), C59(H59A,H59B), C61(H61A,H61B), C63(H63A,H63B),
  C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C16(H16), C32(H32), C36(H36), C44(H44), C64(H64), C68(H68),
 C72(H72), C74(H74), C75(H75), C39(H39), C5(H5), C41(H41), C25(H25), C57(H57),
 C15(H15)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C54(H54A,H54B,H54C), C60(H60A,H60B,H60C), C21(H21A,H21B,
 H21C), C43(H43A,H43B,H43C), C11(H11A,H11B,H11C), C51(H51A,H51B,H51C), C55(H55A,
 H55B,H55C), C31(H31A,H31B,H31C), C65(H65A,H65B,H65C), C33(H33A,H33B,H33C),
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              78697
_shelx_fab_checksum              88759
_platon_squeeze_special_details
;
A solvent mask was calculated and 386 electrons were 
found in a volume of 1633\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1[C7H8], 1[C7H8] per Formula Unit 
which account for 400 electrons per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'