Synthesis and structure of the extended phosphazane ligand [(1,4-C6H4){N(μ-PN(t)Bu)2N(t)Bu}2](4.).
Sevilla, Raquel; Less, Robert J.; García-Rodríguez, Raúl; Bond, Andrew D.; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1868–1871; doi:10.1039/c5dt04393j

data_7037520
_publ_section_title
;
 Synthesis and structure of the extended phosphazane ligand
 [(1,4-C6H4){N(\m-PN(t)Bu)2N(t)Bu}2](4.).
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1868
_journal_page_last               1871
_journal_paper_doi               10.1039/c5dt04393j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C30 H62 N8 P4, 2(C6 H12)'
_chemical_formula_sum            'C42 H86 N8 P4'
_chemical_formula_weight         827.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-04 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                88.944(3)
_cell_angle_beta                 89.034(3)
_cell_angle_gamma                81.094(2)
_cell_formula_units_Z            1
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_cell_length_b                   14.0514(6)
_cell_length_c                   15.4022(7)
_cell_measurement_reflns_used    5146
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      66.01
_cell_measurement_theta_min      4.25
_cell_volume                     1307.93(10)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14919
_diffrn_reflns_point_group_measured_fraction_full 0.986
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_diffrn_reflns_theta_full        66.648
_diffrn_reflns_theta_max         66.648
_diffrn_reflns_theta_min         2.870
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       block
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4576
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1872P)^2^+0.9984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2805
_refine_ls_wR_factor_ref         0.3203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2891
_reflns_number_total             4576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04393j2.cif
_cod_data_source_block           1H4_cyclohexane
_cod_depositor_comments
'Adding full bibliography for 7037519--7037522.cif.'
_cod_database_code               7037520
_cambridge_user_name             'Raquel Sevilla-Martin'
_cambridge_user_crsid            rs617
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RSM74C
_cambridge_data_id               dw_b2_0013
_shelx_estimated_absorpt_t_min   0.712
_shelx_estimated_absorpt_t_max   0.884
_shelx_res_checksum              86949
_shelx_hkl_checksum              70345