Reductive Activation of N2 using a Calcium/Potassium Bimetallic System Supported by an Extremely Bulky Diamide Ligand
Mondal, Rahul; Yuvaraj, K.; Rajeshkumar, Thayalan; Maron, Laurent; Jones, Cameron; Chemical Communications  (2022) –; doi:10.1039/D2CC04841H

data_7130855
_publ_section_title
;
 Reductive Activation of N2 using a Calcium/Potassium Bimetallic System
 Supported by an Extremely Bulky Diamide Ligand
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04841H
_journal_year                    2022
_chemical_formula_sum            'C78.5 H104 K2 N2 O'
_chemical_formula_weight         1169.83
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2czz5j
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-08-31 deposited with the CCDC.	2022-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                113.431(3)
_cell_angle_beta                 99.719(2)
_cell_angle_gamma                97.872(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7093(3)
_cell_length_b                   17.6574(5)
_cell_length_c                   18.1074(4)
_cell_measurement_reflns_used    30686
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      79.7300
_cell_measurement_theta_min      3.5850
_cell_volume                     3580.15(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    xseed
_computing_publication_material  Ciftab
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64002
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         6.570
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             1270
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         13038
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0870
_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^)+(0.1663P)^2^+3.0871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2407
_refine_ls_wR_factor_ref         0.2468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11651
_reflns_number_total             13038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04841h2.cif
_cod_data_source_block           Cj1548
_cod_original_cell_volume        3580.14(17)
_cod_original_formula_sum        'C78.50 H104 K2 N2 O'
_cod_database_code               7130855
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.878
_shelx_res_checksum              61642
_shelx_hkl_checksum              80802