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_7120080
_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
'C44 H86 Ca4 F12 N2 O20 P2 4+, 4(F6 P -), 4(C2 H3 N)'
_chemical_formula_sum            'C52 H98 Ca4 F36 N6 O20 P6'
_chemical_formula_weight         2157.50
_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                100.3963(11)
_cell_angle_beta                 103.0857(11)
_cell_angle_gamma                91.6070(12)
_cell_formula_units_Z            1
_cell_length_a                   12.9890(4)
_cell_length_b                   13.1082(4)
_cell_length_c                   13.8922(4)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.79
_cell_measurement_theta_min      3.44
_cell_volume                     2260.21(12)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26812
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.870
_diffrn_reflns_theta_max         66.870
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    4.348
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       block
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.888
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7970
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+7.5504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7095
_reflns_number_total             7970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc01938f2.cif
_cod_data_source_block           DW_B2_0067
_cod_original_cell_volume        2260.20(14)
_cod_database_code               7120080
_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-2-49
_cambridge_data_id               DW_B2_0067
_shelx_estimated_absorpt_t_min   0.422
_shelx_estimated_absorpt_t_max   0.696
_shelx_res_checksum              88742
_shelx_hkl_checksum              91741