Synthesis of Ca(PF6)2, formed via nitrosonium oxidation of calcium.
Keyzer, Evan N.; Matthews, Peter D.; Liu, Zigeng; Bond, Andrew D.; Grey, Clare P.; Wright, Dominic S.; Chemical communications (Cambridge, England) 53 (2017) 4573–4576; doi:10.1039/c7cc01938f

data_7120082
_publ_section_title
;
 Synthesis of Ca(PF6)2, formed via nitrosonium oxidation of calcium.
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4573
_journal_page_last               4576
_journal_paper_doi               10.1039/c7cc01938f
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety
'C34 H66 Ca4 F10 N2 O15 P 3+, 3(F6 P -), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H72 Ca4 F28 N4 O15 P4'
_chemical_formula_weight         1641.19
_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
;
2017-01-26 deposited with the CCDC.
2017-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                73.456(2)
_cell_angle_beta                 89.794(2)
_cell_angle_gamma                68.867(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7225(6)
_cell_length_b                   13.4339(6)
_cell_length_c                   21.7776(10)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      59.14
_cell_measurement_theta_min      3.75
_cell_volume                     3307.5(3)
_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      180(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0406
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34975
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        59.315
_diffrn_reflns_theta_max         59.315
_diffrn_reflns_theta_min         3.668
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    5.042
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         9471
_refine_ls_number_restraints     426
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+8.9532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8222
_reflns_number_total             9471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc01938f2.cif
_cod_data_source_block           DW_B2_0130
_cod_database_code               7120082
_cambridge_user_name             'Evan Keyzer'
_cambridge_user_crsid            ek406
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             enk-3-9
_cambridge_data_id               DW_B2_0130
_shelx_estimated_absorpt_t_min   0.464
_shelx_estimated_absorpt_t_max   0.633
_shelx_res_checksum              44851
_shelx_hkl_checksum              82374